Trial Exhibit 446 EDTA Lab Sheets and Reports

U.S.
Department of Justice
Federal Bureau of Investigation
Washington, D. C 20s3 5-000
February 28, 2007
Norman Gahn
Calumet County District

206 Court Street.
Chilton, WI 53014
Attorney,s Office
RE: State of Wisconsin v. Steven Averv

Dear Mr.
Gahn:
I am wrJ-ting in response to a letter f rom rlerome F.

Buting dated February 25, 2007, reguesting discovery in the
above-captioned matter. Eacrh request relating to the analysis
performed by the FBf Laboratory is addressed individually bel-ow.
1.
"The protocol issu.e date is February 1_5, 2007...,
Enclosed is a copy of the relevant analysis
protocols utilized by the FBI Laboratory in this case.
2.
"Any data on tests the FBI has done or cuIled... ',
There were no tests performed by the FBI that
determined the amounts of EDTA found in ordinary
household or automotive objects.
3.
"Any and all lab sheets, work sheets, bench sheets. .,,
Enclosed is a copy of al-I of the fite material
generated by the FBI Laboratory relat,ing to the
analysis performed in this case. This material
incl-udes bench notes, computer printouts, chain of
custody documents, and all other specific information
regarding the case. A CD Rom is also included with
this materiaL containing raw data files. These fires
cannot be accessed unless the proprietary software
which is available from Thermo Finnigan, is installed
on your computer.
{^r 4'l l(i )
"*,a3{60TL
"l\ny and all valiclation studies the FBI has done.
4.
.,,
Enclosed is a copy of the validation studies.

"Any and alL "limltation of detection" studies. . .,,
5.
Information regarding studies referred to in the

protocol in this case is found in the material provided
for response 4.
"Any and aL1 "selectivity"
5.
st,udies referred to in...,,
Information regarding studies referred t.o in t.he

prot.ocol in this case is found in the material provided
.,
8.
t_0
1L.
for response 4.
"Any and all "matrix effects" studies referred to...,,
Information r:egarding studies referred to in the
protocol in this case is found in the material provided
for response 4.
"Citations to any and all "literatrlre" referred to. ."
Information r:egarding literature referred to in
the protocol j-n ttris case is found in the material
provided for response 4.
"A list of any ancl all cases where Marc LeBeau. ."
Inasmuch as this request if not for documentation
relating to the pz:esent case or for documentation
regarding underlyj"ng scientific data, it is beyond the
scope of discovery.
"A complete curriculum vitae for any individual. . "
The analysis in this case was performed by Unit
Chief Marc A. LeBe:au. Chemist .fason Brewer was the
Technician. Examiner Madeline Montgomery was the
Technical Reviewer and Examiner Eileen Waninger was the
Administrative Rev'iewer in this case. A copy of their
curriculum vitae i.s enclosed.
"A1l data reflecti,ng the rate of degradation or..."
fnasmuch as t.his reguest is not for documentation
relating to the present case, it is beyond the scope of
dj-scovery. This information can be researched by any
defense expert and is in the public domain.
2
^t, +4 b
ro)
1,2.
13.
L4
15.
"Any complaints or negative performance evaluations. . .,,
Pursuant to IIBI Policy, a review of t,he Examiner,s

file for complainl-s or negative performance evaluations
may be requested in writing by the prosecutor to t.he
appropriate Chief Division Counsel, who will coordinate
a search with appropri-aLe legal personnel at
HeadquarLers. Laboratory personnel may not have access
to certain personnel files containing such information.
"Any and all insicle or outside prof iciency tests. . .',
A copy of Lhe completed proficiency test summaries
Unif
for
Chief Marc A. LeBeau, Examiners Eileen
Waninger and Madeline Montgomery and Chemist ,Jason
Brewer is enclosed.
"Laboratory chain of custody records, including a1I..."
A11 informatlon, regarding chain of custody of
evidence for this case will be found in the case notes
provided for response 3.
"Copies of traceability documentation for sEandards. . . "
A11 informatjlon regarding traceability for this
case will be founcl in the case notes provided for
response 3.
15.
"Instrument run 1og with identification of aII. . . "

A11 informati-on, regarding instrument run logs for
this case will be found in the case notes provided for
response 3.
L7.
"Records of instrr.rment maintenance status and..."
Enclosed is er copy of the maintenance records of

t,he j-nstruments used in the analysis of this case, for
t.he time period surrounding the examination in this
arz c!a
18.
"An error or contamination 1og covering any and a1l..."

There were no instances of contamination in this
case. Had any instances occurred, the documentation,
including actions taken, would be included in the
material provided in response to request. 3. Any
request for documentat.j-on regarding error or
fa ++t'
( 3)
contamination that occurred in other cases is bevond

the scope of the discovery.
1-9
"Raw
data f or the complete measurement sequence. . . ,,
A11 information regarding the raw data for this

case, is found on the CD provided in response to
request, 3.
r hope this materi.al will assist vou in this effort.

,Joseph DiZinno, D.D.S
Assistant Director
Laboratorv Division
by
lfit tL. .//lI
/rr
'f
/ Robert Tram
Section Chief
Scient.if ic Analysis Section
Enclosures
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150
0?,28107 05:51:47
BTANK (neg blood, Dl H2O ext.)
NL:0
r.l=
272.9273-5 F: - c
ESI SRM ms2
291.20@15.001
246.50-247.50,
272.50-273.501. MS
STAEILITYOS
ffilz. 248.+217 .5 Ft - c
ESI SRM ms2
291.20@15,00 [
246.50-247.50,
272.50.273.501 MS
m/2.325.5-326.5 F: - c
STABILITYOS
STABILITYOS.
ESI SRM ns2

341.20@15.0O I
299.50.300.50,
325.50326.501 MS
itc
2
o
Time (mh)
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*-l
*-l
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NL: 2.46E3
rlT-246.5-241,5 F: - c
rYF 325.$326-5 F: - c
ESISRM rc2
291.20@15.00 I
246.50-".47.50.
272.50-?73.501 MS
STAEILlrYog
ESI SRM ms2

314.20@15.00 t
299.50-300.50.
325.50-326.501 MS
STAAILITYO9.
8G
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60-.1
(0I
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02128tO7 06:13:31
NL:0
tnlz=272.1273,5 F:. c
rrlz= 299.$300.5 F: - c
ESI SRM ms2
ESI SRM ms2

29t.20@15.001
246.50-247.50.
272.50-273.501 MS
STABILITYIO
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02128107 06:24:27
0
nlz= 272.1273.5
BLANK (neg blood, Dl H2O ext.)
NL:
F: -
ESI SRM ms2

291.20@1s.oo I
246.50-247.*,
272.5C273.501 MS
STABILTryI I
r/z= 325.S326.5 Fi. c

ESISRM
N2
344.20@15.001
299.50.300.50.
325.50.326.501 MS
STABILTTYI
o
6
NL:
nlz-282.&284.3FtESI SRM
ns2
303.20@1s.001
282.7$2134.251
STABILNYIl.
Timc (min)
MS
LrV
/q\
C:U(calibuA...\Stability\Stabilityl 2
1001
try'F 325.5-326.5 F: - c
ESI SRM ms2
s5-.1
34.20@1s.00 [
.o-]
299.50-300.50.
325.50.326.501. MS
STAEILITYl2
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80-j
zs-]
?o-l
uu-l
8
Fr
60-.1
\o't
mn= 282-8-2u.3 F: - c
ESI SRM msz
303.20@1s.o0l
282.75.2{1.r.251 MS
sTAA[ttYt2
,{ vr
(
i",)
:\)(calibuA...\Stability\Stabilityl
02128107 06:46r08
NL: 0
mlz= 272.5-213.6 Fi - c
ESI SRM ms2
NL:3.80E3
m/z= 299.$300.5 F:
ESI SRM rE2
344.20@15,00 I
291.20@15.001
246.5&247.50,
272.50.273.501 MS
299.5G300.50.
325,50-326.501
sTA8tLtryl3
STABtltryl3-
NL: 0
r]/z= 24A.5-247.sFi. c
ESI SRM ms2
291.20115.0O
246.50,247.50,
272.50-273.501 MS
STABILIryl3
'llma (mln)
,4q
(,,\
Tlne (min)
MS
.c
:U(calibur\...\Stability\Stabil
ity
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0212U07 06:57:01

NL:0
NL:0
ntz=272t.U?73.5F',. c
nt.|:= 299.5-300.5 F:
ESI SRM ms2
ESI SRMms2
29r.20@ rs.0o I
246.50-247.50.
272.sG273.501 MS
STABILITY,I4.
34420@1s.00
.c
299.50-300.50.
325.50326.sO1- MS
STABILITY1,I
rVF 325.5326.5 F: - c
ESI SRM ms2
34420@15.0O I
29S.5G300.50,
325.5S326.501 MS
SIABILTTY,I4-
is
oe
lo
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rnlz=282.9.2U.3F:- c
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ms2
303r0@'15.00 [
282.7U28l
',t MS
STAB|L|Y14'
nm
(nin)
t{ qk
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Tirne (rnh)
C:D(calibur\...\Stability\St bilityl 5
Card C extract (EDTA +)
NL:4,61E4
100-l
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0?i28107 07:07:51
Nz=272.*273-5 F: - c
ESI SR[,] ms2

29r .20@15.00
246.50-247.s0,
272.50-273.501 MS
so"]
STAEILITYIs-
NL:1.06E,1
ntlz.216-5247.5F: - c
ESI SRM ms2
2s1.20O1s.00
246.n-247.fi-
mfu:325.5-326.5 F: - c
ESI SRM ms2
344.20@1s.00 [
299.50.300.50.
325.50.326.50t- MS
272.5S,273.501 MS
sTABtLtrYlS'
sTAErUTYls
rlz=
282.9-284.3F: - c
ESI SRM ms2
303.20Ots.@ [
282.7$2r(.251- MS
STABILITYl5
Tme (min)
C:Xcalibur\...\Stability\Stabilityl
159
0?/28107 07:18:40
BLANK (neg blood, Dl H2O
NL:0
n!z'272.5-273.5F: - c
m/z= 299.$300.5 F: - c
ESI SRM ms2
344.20@15.0o l
ESI sRM ns2

29120@15.00 [
246,5e247.50,
272.5G?73.501 MS
299.5&300.50.'
325.50.326.50t Ms
STAEILITY16'
STABILITYI6.
rn/z= 245.$247.5 F: - c
ESISRM ru2
291.20@15.00 [
24650-?47.50,
272.50-273.501 MS
STABIL|TYI6
a
E
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Tim
(min)
exl)
Tim
(mln)
:U(calibur\...\Stability\Stabilityl 7
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02128107 07:29:35
NL:
tnlz= 272.5-273.5 Fi . c
ESI SRM ms2
291.20@15.00 (
216.fi-217.fi,
272.50-273.sot MS
sTABtLtrYlT'
nlz- 246.5.247.5 F: - c
ESISRM ro2
29120@15.0O I
216.5G217.fi.
272.50-273.fit US
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0228107 07:40:31
Card D extract (EDTA
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NL:1.14E5
tnJl.272.9273.5 F:- c
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291.20@1s.001
246.5S247.50,
272.5G273.s01 MS
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rn/z: 325.$326.5 F: - c
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3{4.20@15.0O I
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rnlz= 282.8.2U.3F:. c
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303.20@ rs.00 t
282.7$2114.25t MS
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STA8ILITY18.
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t"oqo
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311.9,3'12.5 F: . c
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356.00@1s.oo I
311.5&312.501- MS
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0212W07 07151:26
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BIANK (neg blood, Dl H2O ext.)

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ntlz= 272.1213.5 Fi - c
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ESI SRM msz

341.20@1s.00 t
291.20@15.00 I
246.50-247.50,
272.50-273.s01 MS
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r|/!= 24i.$247.5
299.50.300.50.'
325.5e326.501 MS
STABILITYl9
F: - c
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29r.20O15.@ [
246.50-247.50.
272.50-273.501 MS
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299.5.300.5 F: - c
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02128107 08:02:20
NL:0
tr!z.272.5-273.5Fi
ESI SRU ms2

29120@15.00 I
246.50-it47.50,
272.s0.273.501 MS
STAEILITY2O
rvz= 325-$.326.5 F: - c
ESI SRM ms2
344r0@15.00 {
299.5&300.50,
325.50.326,s01 MS
STABILTTY2O.
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29120@15.001
216.*247_fi.
272.5G273.50t. MS
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303.m@rl5.m I
282.7$234.251 MS
STABILI|Y2I
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02f28rc7 08:24:05
<-
NL:0
tlz-272.5.273.5F:.
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ESISRM m2
34.r.20@15.001
299.5G300.50.
29'r.20@15.0O I
245.5G247.50,
272.50-273.s01 MS
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u5.5G326.501 Ms
STABtLrry22'
trVz=
325.S326.5 F: - c
ESI SRM ms2

344.20(D15.0O I
299.50.300.50,
325.5G326.501. MS
STABILITY22
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6
4
nn (rin)
li,
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C:\j(calibur\...\Stability\Stabllity23
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0?i2407 08:34:58
BIANK (neg blood, Dl H2O ext)
Nti 0
nlF272,*273.5 F:.
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c
nvz= 299.t3@.5 F: - c
ESI SRM ms2
341.20@15.00 t
ESI SRM ms2
291.2001s.00 [
246.5G247.50,
272.5G273.50t MS
STABILITY23.
299.50.300.50.-
325.50.326.5O1 MS
sTAEUryA'
nlz-
246.5.247 .5 F: - c
ESI SRM ms2
291.20@15.00l
246.5e2{7.50.
272.5e273.501 MS
STABtLnY23'
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02f28107 08:45:49
Card F extract (EDTA +)
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1
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282.7$284.25t MS
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02128107 Q8:56:43
NL:0
tnlz= 272.$273.5Fi - c
ESI SRM ms2
291.20@15.00 I
246.50'247.50.
272.5G273,50t MS
STABILIT\2s.
n/z:325.$326.5
F:
ESI SRM ms2

3,t4,20@15.00 [
299.50.300.50.
325.50.326.501 MS
STABILITY2S.
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C:XcalibuA...\Stabillty\Stability26
D2l2U07 09:07:38
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NL: 0
rNL= 272.5-273.5 F: ESI SRM
rE2
291.20@1s.00 [
245.50-2,t7.50.
272.50-273.501 MS
STABILI-IY26
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rYz.3l't.$312.5
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356.00O15.00 [
311.5e312.501 MS
STABILITY26
Tim
(min)
8r44,
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C:U(calibuA,..\Stability\Stability2T
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02f28107 09:18:28
Card G extract (EDTA +)
NL: 7.78E,1
t*-l
-c
rnlz=272.5.273,5F:
esl SRM ms2

2s1.20or 5.0o (
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2,r6.5S247.50,
272.50-?73.501 MS
STABILIW2T
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NL: 6.333
rr/F
246.5-247.5 F: . c
ESISRM ru2
29r.20O1s.m I
246.55247.50.
299.5G300.s0.
325.5G326.501
. MS
272.5G273.501 MS
STASILITY2T-
STAEILITY2T
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nlz.2V..8-N.3F:
ESI SR { ms2
30320@ r5.00 [
282.7$284.25t MS
STABILITY2T.
Tlmr (rnh)
rnr:= 325.5-326.5 F: - c
ESI SRM msz
34,120@15.@ I
-1h?
:U(calibuA...\Stability\Stability2S
02128107 09,29:23
NL: 0
tnlz=27?:..5.2f 3.5F: - c
ESI SRM rts2
rn/2" 299.5.300.5 F: - c
ESI SRM rrE2
29120O15.00 [
34420015.00I
246.5G217.50.
272.50-273.501 MS
sTAEtLnaa2S'
299.50-300.s0.
325.5o326.50i Ms
STABILITY2E-
4,5283
ttlz.248.*247.5
ESI
Fi - c
tdz.325.5.326.5 F: - c
SRil ms2
ESI SRM ms2

34420@1s.oo l
299.50-300.50,
325.s0-326.501 MS
2e120@15.00 [
246.50-2,t7.50.
2r2.so-2r3.soi Ms
STA8[lIY2E
Tm
(nin)
STABILTN/28
Tlme (rnln)
:U(calibur\...\Sta bility\S tability29
02/28107 09:40:17

NL:2,90E3
rnrz= 299.5.300.5 F: . c
'*'r
e51
ESISRM
ro2
34.20@r5.001
so'l
299.50.300.50,
325.50.326.s01 Ms
STABILITY2g'
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t
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o
ftlz'2A2.6-284.3F:. c
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3O3.20(!1 s.00 I
262.7'|A1.A1
MS
STABILITV29.
Tinr (rin)
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Ti.ra (min)
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'*l
-l
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*l
Tuf
A2128107 09:51:06
rnlz. 246.1247 ,5 Ft - c
ESI SRM ms2
291.20@15.00 [
Card H exbact (EDTA +)
nvz:325.5-326.5 F: . c
ESI SRM
c2
34420@rs.00 [
216-5n.217 -5o.
299.50.300.50,
272.50.23.501 MS
325.5S326.501 MS
STABILIry3o
STABILTTrcO
uo1
'-l
zo-l
,a-l
*l
\oI
311.$312.5 F: . c
ESISRM m2
f,r/u =
3s6.00@1s.oo
311.5G312.501 MS
STABILITY3O'
,C,
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+q
l,
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:Xcalibur\...\Stability\Stability3
J-D$
A2128107 10:01:55
BLANK{neg blood, Dl H2O ext.)
NL: 0
nlp 272.U273.5 F: - c
ESI SRM ms2
2s1.m@15.00 [
246.50-247.s0.
272.50-273.501. MS
STABILITY3I
ftVz= 2,16.5-247.5 F: - c
ESI SRM ms2
291.20@1s.@ [
246.5o.247.50272.5e273.s01 MS
STABILITY3l
o
o
-E
e
E
r/z=
31
.9312.5 F: -
ESI SRM ms2

356.00@1s.00 [
311,5S3'12.501 MS
STABILITY3l
Tinr (dn)
q+l
t) ^n,\
/
nnrc (tiln)
'-
C:U(calibuA...\Stability\Stabilitv32
Tb{
0?i28,C/ 10:12:51
NL: 0
fii1F272.5-273.5 F. - c
ESI SRM ms2
291r0@r5.00 [
246.50.247.50.
272.50.273.501 MS
STABILIIY32
dtlzE 216.5247.5 F:
ESI SRM trt32
.c
291.20@r5.@ I
246.50-247.50,
272.5G273.501 MS
STABILI']Y32
t
e
o
It
2.138A
ilz= 282.U28/..3F:.
ESI SRM
ns2
3O3.20O15.@ [
282.75.2t14.25t. MS
STABILTTY32
40
Tim (;'in)
C:Xcalibu 4...\Stability\Stability33
-J uP
0428107 10:23:40
Card I extract (EDTn +;

NL: 9,55E4
nvz= 299.5.300.5 F: - c
ESI SRM ms2
tr'lz=272-5-273.5 F: - c
ESI SRM ms2
;:::,39;iS,{
272.50-273.501 MS
344.20O15.001
299.50.300.50.
325.50.326.501 MS
STAEILITY33
STABILITYS.
,*l
rTri:=
'l
ro-]
299.50-300.50.
32s.so-326.50i Ms
rul
sTABtLtTY33'
,o-l
'l
ro-l
65-J
325.5-326.5 F: - c
ESI SRM ms2
344.20@1s.00 |
eo-.]
$l
tlF
282.&2U.3 Fi - c
ESI SRM ms2
303.20@r5.00 [
282.7$21425t MS
STASILNY$.
{'o +al
Tim (min)
:Xca libuA...\Stability\Stability34
-l oF
02128/07 10:34:32

NL:2.4OE3
tr/z= 299.$,300.5 F: . c
ESI SRM ms2
34420@15.00 |
299.5G.300.50.'
325.5G.325.50t MS
STAEILITYs4'
n/2- 246.$247.5
F: ;
ESI SRM ms2
291,20O1s.@ [
246.fi-217.fi.
272.50-273.501 MS
sTA8rLfry34'
o
9
,l
E
o
E
o
ll'
10(
g
s[
8(
7l
6{
45
40
1(
TirB (n{n)
{lo,aap
Thn. (min)
aiF
C:u(catibuA,,.\Stability\Sjqj!!ty35
0?i28107 10:45:25
NL:1.94E3
lxt:
BTANK (neg blood, Dl HzO ext.)
u.utj . 19.u2 5M: 3(i
nlz=272.5-273.5 Fi. c
ESI SRM ms2
291.20Or5.001
246.50-247.50.
272.5S273.501 MS
STABILIry35.
r!z=216.5-247.sFi- c
ESI SRM ms2
29120@15.00 [
216.*247.fi.
272.sS273.501 MS
STABILITrcS'
o
d
e
o
-!
rfilz= 292.t12E4.3 F: - c
ESI SRM irs2
303.20@1s.001
2&..7r2U.25t-
MS
STABILIT}'35
Tim
lmin)
nm(nrin)
0212407 10:56:17
'*-.l
nlz- 272.$27!.5
-l
291.20Or5.00 [
Card J extract (EDTA +;
F: - c
ESI SRM ms2
95-.1
246.50-247.50.
272-50.273.501
MS
STABILI1Y36.
10o-l
rvz= 325.5.326.5 F: - c
,5.1
ESI SRM ms2
34420@rs.00l
*1
299.5G300.50.
325.5G326.50t MS
STABILITY36.
ru']
80-..1
'u-]
'o']
uu-l
*.1
fimG (rim)
t:*++tu
Tln (nin)
A2l2U07 11:07:10
:[(calibuA...\Stability\Slability3T
BIANK (neg blood, Dl H2O exl.)
NL:0
trlz- 272.$273.5
F: -
flVz=299.$300.5 F: - c
ESI SRM ms2
ESI SRM ms2
34420@1s.001
29120@15.001
299.50.300.50,
325.50-326.501- MS
216.fi-247.50.
272.50-273.501 MS
STAAILITY3T
sTABtLnr3T
n/z'
31 1.5-312.5 F: - c
ESI SRt4 ms2
3s5.00o1s.00 [
311.50-312.501 MS
STAEILITY3T
(-y
++('
Tm(min)
-jlF
C:U(calibur\...\Stabilih^Stabilitv3E
t*r
0?/2U07 11:18:05
NL:
rul
2.16E3
NL:1.55E3
rtlz?272.12?3.5F: -c
r/z= 299.$300.5
ESI SRM ms2
ESI SRM ms2

3.+4.20@15.00 I
291.20@15,00 [
246.50-247.50.
e0-l
299.50.3@.50.
32s.50-326.50t MS
2t2.50.273.501 MS
STAB|UW3S'
sTAEtLrTWs'
gE
!t
.l
.E
Ilr.
(min)
J.'.oa'l
ltu)
F: - c
Tim
(ndn)
100 ppm EDTA
,*-l
ru-l
s0l
tol
rv.= 325.5-326.5 F: - c
ru-l
ESI SRM ms2

34,r.20@15.001
,o-j
299.5&300.50.
325.s0.326.s0t MS
STABILITY3g.
85-]
ro-]
rrl
ro-]
*'l
*-l
I'lz-2a2.8.2U,3Ft. c
ESI SFIM
tr82
30320@1!;.001
282.7$28.1.2q MS
STABILITY39
nrulmin)
{r f:,K
0?/2U07
1:39:48
NL; 0
nlzr 2f2.s273.5
F; - c
ESI SRM ms2
29120O15.001
248.*21f .9,
272.5G273,501 MS
STABILITY4O
Tlm(mir)
BLANK (neS blood, Dl H2O ext.)
:l(calibuA...\Stab ility\Stability4
TbF
BLANK (neg blood, Dl H2O ext,)
0228[07.11:50:40
u.oo -
RI:0.00-10.02 SM:3G
NL:
ru.uz sM: rG
lr<r:
tilz=272.*273.5Fi - c
ESISRM
ruz
NLO
rn/z= 299.t300.5 F:
ESI SRM rsz
.c
29120@r5.00 [
24650.247.50,
l#:"38J3.S,t
272.50273.501 MS
STABILITY4I
325.50-326.50t- MS
STABTLITY4'I
tr'lz=246.6247.5F: - c
nvz:325.$326.5 F: - c
:2.06E3
ESI SRM rns2
29r 20O'r 5.00
ESI SRM ms2
li3:338J333t
246.50247.50.
272.50273.501 MS
STABILITY4l
32s.5G326.501 MS
STABILITY4T
o
?
i
o
io
rr'z= 2a2.&-2E/.3 F: - c
ESI SRM rns2
30320@t s.00 [
282.75-2eQ51 MS
sTABtLrn'41
{*
L4 to
,-
0A28107 03:31:28
:U(calituril..\EDTA\Brewer\O22807U2801
NL:
EDTA neg blood/H2O extract
To{
NL:2.55E3
nlF n2,*7135Fi-
rn/z:290.$300.5 F: - c
ESI SRM rns2

311420@1s.001
299.50-300.50.
ESI SRM nE2
291.20@,|5.00 [
246.9.241.fi.
32s.sG326.5O1 MS
272.50.273.501 MS
22001
22fJJ1
nJZ.216.*217,5Fi - c
ESISRM ffi2
29r20Ct15.0O I
246.5G247.50.
272.5O-Zr3.5Ol MS
2?@1
!
c
:r
{3
.t
.9
nft= 311.$312.5
F:
ESISRM G2
356.00O1s.00 [
3r 1.5G312.sO1 MS
22Eo1
Ifm ln{n)
Cr
Tlm(rnn)
+q
:l(caliDuA...\EDTA\BreweA022807tE,2B02
0A28107 03:42i41
100 ppm
EDTA
'--ir D
J'f
NL: 1.56E4
rof
m/r:299.$300.5 F: . c
nl
ESI SRM ms2

344.20@15.00 I
299.50.300.50.
*-1
325.50-326.sot MS
22802
*-l
m/:= 325.5-326.5 F: - c
ESI SRM ms2
34420@15.00 [
nJz= 24Ei.5.217.sFi - c
ESI SRM ms2
291,20@15.00 [
246.5(F217,50.
272.5G273.so1 MS
22802
299.50-300.50,
325.50-326.501
MS
22802
8oo
tuu
e
.:o.
o
m/2.311.$312.5Fi-c
ESI SRM ms2
356.m@15.0O I
311,5O.312.501 MS
22eo2
Tim(mh)
Seq
uen
ce---E DTA-sta
bi
ity-n eg ion sld [O pen]

.
Sample Name: BI-ANK (neg blood, Dl l't9o ef.)n

Study:
Comment:
Client
Laboratory:
Company:
Phone:
Xcal
bu
Amethod s\EDTA_Neg_
Sample Name:
Comment
Study:
Client:
Laboratory:
Company:
Phone:
Sample Type File Name
Sample lD
Unknown
STABILITYO2 02
Proc Method
CalFile
Position
1
Inst Method
Path
C
:\Xcalibu tlData\E DTA\Brewer\Stability
njVol
5.0
Level
u:\
GilrDunmemoos\Eu I A_Neg_swaDs
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
1.000
ozl..xl't
SF
Seq uence--E DTA-sta

Sample Name:
iI
ity-neg on. s d [Open]

i
card extract
Study:
Comment
Client
Laboratory:
Company:
Phone:
Sarnple Type
ile Name
Sample lD
Unknown
STABILIryO3 01
Proc Method
CalFile
lnst Method
Path
:\Xcalibu nData\EDTA\Brewenstablllty
Position
lnjVol
5.0
Level
C:
U(calibur\methods\EDTA-Neg-Swabs
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
1.000
(neg blood, Dl H2O ext,
Sample N
Study:
Comment:
Client
Laboratory:
Company:
Phone:
Sample lD
Path
lnst Method
C
Unkno,vn
STABILITYM 01
C:Xcalibu AData\EDTA\BreweAStability
Proc Method
CalFile
Position
lnjVol
5.0
Level
:Xcali bu r\methods\E DTA_Neg_Swabs
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
1.000
otlt-rl"t
Seq u en
ce-- E DTA-sta
bi
ity-ne g ion. sl d [O pen ]
(neg blood, Dl H2O ext.
Sample Name:
Study:
Comment:
Client
Laboratory:
Company:
Phone:
Sample lD
Unknown
STABILIWOs 01
Proc Memoo
CalFile
Position
1
lnst Method
Path
C
fXca[i ou rtOata\EDTA\Brewer\Stability
Level
njVol
5.0
:Xcali bu r\m ethods\EDTA-Neg-Swa bs
Sample Wt
Sample Vol
ISTD Amt
t.000
0.000
1.000
ffifrffiisffittrffiatt*fttffifftffffitffittffiffiatlffilillta*tttttt#ittltt*tffifftttill*iit*txlfft'ttttft
Sample Name:
I
comrnent
studY:
Client:
Laboratory:
Company:
Phone:

Unknown
lDil
Factor
Sample lD
STABILITYO6 01
lnst Method
Path
C
:\)(calibu r\Data\E DTA\Brewer\Stabili$
:v(calibur\metnocls\ts
IJ I
A_Neg_swaDs
n006---l
rttatt*tt**frtt**tt**hitttttittt*iaftittit*t*t**Ht#fr
tat*frit*tF6l*ttrt*HttttftffaitlttattHat*ttttffti*trattrtifffft*ta*tt
f; q+\
{r/
(
page
e,
otftl"t
'ft?
Seq uence---E DTA_sta bi I ity_neg

Sample t,tame:
o n. s
ld
[O
pen]
tl
Study:
Client:
l-aboratory:
Company:
Phone:
Sample lD
Unknown
STABILIryOT 01
g:
Proc Method
CalFile
InjVol
Position
Inst Method
Path
u(caltbunDaE\ts D I A\Hre\r/er\Stabrlrty u:xcallbunmemods\tsD I A_Neg-liwabs
Level
5.0
Sample Wt
SampleVol
ISTD Amt
0.000
0.000
1.000
Sample Name:
Comment:
Study:
tllient:
l-aboratory:
Oompany:
Phone:
sample lype File Name
Sample lD
lnst Method
Path
Unknown
STABILITYOS 01
C:XcaliburlData\EDTA\BreweAStability
Proc Method
CalFile
lnjVol
Position
Level
5,0
+s1
\Xcalib
r\m ethods\EDTA_N eg_Swabs
Samole Wt
Sample Vol
STD Amt
3.000
0.000
1.000
[* +na
page4'
ovl*1"1
{!P
Seq
uen
ce---E DTA_sta bi
itlneg
on . sld [O pen ]
+)
Sample Name:
Study:
Comment:
Client:
Laboratory:
Company:
Phone:
Sample lD
Unknown
STABILIWOg 01
Proc Metnod
CalFile
Position
Sample Name:
neg
lnst Method
Path
C
:\)(calibuAData\EDTA\BreweAStabili$
njVol
Level
5.0
:U(cal i bu r\m ethods\E DTA-Neg_Swabs
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
1.000
Comment:
Study:
Client:
Laboratory:
Company:
Phone:

Unknown
Sample lD
STAEILITYlO 01
lnst Method
Path
c: \xcali bu
RDaIa\EDTA\B rewer\Stability
r'(L,
fr qL,\
page 5
C :\Xcalabu
r\methods\E DTA_N eg_Swabs
ouluel"l
.S.roF
Seq
uen
Sample Name:
ce--E DTA_sta
iI
ity_n eg ion
[O pe
ext.
Study:
Comment:
Client:
Laboratory:
Company:
Phone:

Unknown
STAEILITY1l
Proc Method Cal File
Sample lD
01
Position
lnst Method
Path
:U(cal i bu AData\EDTA\Brewer\Stab
InjVol
Level
5,0
Name:
IJ
Comment
Sample
ility C:XcdibuAmethods\EDTA_Neg-Swabs
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
1.000
Study:
Client:
Laboratory:
Company:
Phone:

Unknown
ttaaittttt*ff
Sample lD
STABILITY12 01
lnst Method
Path
u:\
cattDunuata\Eu I A\tsrewen$EDilrty C:\Xcalibur\methods\EDTA_Neg_Swabs
tttittttit*t*
fl,t+a
(v
page
t)
6'
or-
urJ"'l
'{nP
Seq uen ce---E DTA-sta bi ity-neg on . sld [O pe n]

I
Sample Name: BI-ANK (neg blood, Dl H2O eX.

Study:
Comment:
Client:
Laboratory:
Company:
Phone:
Proc Method
CalFile
Position
InjVol
5.0
Level
Sample Wt
Sample vol
ISTD Amt
0.000
0.000
1.000
Sample 11366'
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
STAEILITYl4
01
Proc Method
CalFile
Position
Injvol
5.0
lnst Memod
:Xcalibu r\Data\EDTA\BreweAStabili$
Level
5. qu"
( as)
pageT'
:Xcalibu Amethods\E DTA_N e g_Swabs
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
1.000
orlrsl-t
'gP
S eq u ence--- E
DTA-stab ity-neg
i
o n.
sld [O pen]
Sample Name:
Comment
StudY:
Client:
Laboratory:
Company;
Phone:
Sample lD
Inst Method
Path
Unknown
STABILITY1S 01
C:U(cali bu r\Data\EDTA\8 rewe r\Stabi lity
Proc Method
CalFile
Position
InjVol
5.0
Sample Name:
(neg
Level
:Xcalibur\methods\E DTA_Neg_Swa
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
1.000
bs
ext.
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
SamDle lD
Path
lnst Method
Unknown
STABILITYl6
01
c: u(caltDu r\Data\Eu I A\tsrewensEDrlrty
Proc Method
CalFile
Position
InjVol
5.U
Level
[*'/'/-,
( +q\
page
8/
:\Xcalibur\methods\EDTA_Neg-Swabs
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
1.000
orl*1.1
,s,P
Seq
uen
ce-- E DTA-sta
iI
ity-neg
io n. s I d [O
pen]
neg blood, Dl H2O ext.)
Sample Name:
Study:
Comment:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
lnst Method
Unknown
STABILITYlT
01
C:\)(calibuAData\EDTA\BreweAStabil
Proc Method
CalFile
Position
InjVol
5.0
Level
ity
Xcalibur\methods\EDTA-N eg-Swabs
Sample Wt
Sample Vol
ISTD AMt
0.000
0.000
1.000
trffiffiffiffiffif,*tftl*'t*llffftltf.ttttffi**tttlllttttttt.ttffltffitftsfrttlllltaftt*tt.tta
Sample Name: Card D extract (EDTA +

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
5z,tu+
/5o)
9'
page
o.lrrl't
'av?
S eq u ence--- E
DTA-sta
bi
ity-n eg
o n.
sld
[O pe
(neg blood, Dl H2O ext.)
Sample Name:
Study:
Comment:
Client:
Laboratory:
Company:
Phone:
Inst Methotl
Sample lD
Sample Type Fild Name

Unknown
STABILITY19
01
C:Xcali bur\Datra\EDTA\Brewer\Stability
Proc Method
CalFile
Position
lnjVol
5.0
Itiff
rtrttff
tffi
Sample Name:
Comment:
ffi
F.tttff
tlttl*llt#tltttrtff
ttft$tff
Level
lllff
lfr tltAttltff
:Xcdibu Amehods\E DTA-N eg-Swabs
Sample Wt
Samole Vol
ISTD Amt
0.000
0.000
1.000

Study:
Client:
Laboratory:
Company:
Phone:
foquo
( s,)
page'10
ovlt'||t"1
'$'P
EDTA Stability Study:

Ten EDTA-preserved blood spot cards were analyzed following approximately 33
months of storage at room temperature. The free acid form of EDTA was detected in all
l0 of the spot cards. The EDTA-iron complex was detectable in 6 of the l0 spot cards.
Failure to identify the EDTA-iron complex was based on the lack of the less abundant
product ion (m/z 326). The more abundant m/z 300 for EDTA-iron was present in all l0
ofthe spot cards.
5o +v6
G4
CASE FILE
t,
q+b
(')
7;l-M*a'ct.t6)
ffiffi'@
2501 Investigation Parkway

Quantico, Virginia 221 35
REPORT OF EXAMINATION
To: Milwaukee
Date: Febru ary 26,2007
Squad 6/GBRA
SA Gerald E.
Mullen
Case
Lab
Reference
: Communication
IDNo.: 62D-MW-443$*bl
No.: 070201013 PM GH
dated January 3 0, 2007
Your No.:
Title:
STEVEN AVERY;
TERESA HALBACH-VICTIM (DECEASED)
DOMESTIC COOPERATION-HOMICIDE
Date specimens received:
February 1,2007 arrd February 6,2007
The following items were examined in the Chemistry Unit:
Q46
Swab (Item 9569)
Q47
Swab (Item 9574)
Q48
Swab (ltem9572)
Q49
Liquid blood sample from STIIVEN AVERY (Item 9803)
K2
Two control swabs (Item 9802)
K3
K4
This report contains the results of the chernistry examinations.
Page 1
of3
For Official Use Onlv
14t6
(
s+\
Results of Examinations:
Specimens Q46-Q49 and K2-K4 were analyzed for the presence of ethylenediaminetetraacetic acid @DTA).
Specimen Q49 was listed as a liquid blood sample from STEVEN AVERy in a l0
5.5 mL of blood. EDTA was
identified in specimen Q49.
milliliter (mL) lavender-top blood tube. It contained approximately
Specimens Q46-Q48 were reported to be collection swabs of blood stains from

the
crime scene associated with the death of TERESA HALBACH. Specimens K2-K4
were reported
to be control swabs collected in relation to the Q46-Q48 swabs. BO1R, either as the free
acid or
as the EDTA-iron complex, was not identified on the
e46-e4g or K2-K4 swabs.
The analysis for EDTA was carried out using liquid cluomatography/tandem mass
spectrometry in both positive and negative electrospray ionization modes.
Remarks:
EDTA is an anti-coagulant and en4rme inhibitor that is commonly used in blood
collection tubes. Blood specimen collectiorr tubes containing EDTA have lavender-colored tops
and are the most common collection tube used to collect reference specimens for DNA testing.
The concentration of EDTA in its free acid form in a drawn blood tube is typically
1000-2000 milligrams per liter (mg/L), depending on the volume of blood and the.up*ity
oith.
tube. At this concentration, the free acid and salt forms of EDTA are soluble in blood. EDTA
readily forms water-soluble chelates with nearly all heavy metals, including iron in blood.
Aqueous extractions of dried bloodstains allLow for the isolation of EDTA (both as the free
acid
and as the EDTA-iron complex) if present.
Using the procedure employed irr this case, EDTA is readily identified at a
concenfration of 13 mglL. Additionally, ELITA is also detectable when a 1-microliter drop
EDTA-preserved blood is analyzed
of
For questions about the content of this report, please contact Unit Chief Marc LeBeau
(703)
at
632-7408.
Page2 of3
07020t013 PM GH
o ++e,
1st)
For questions about the status of remaining forensic examinations,

please contact Request coordinator Michael vanArsd-ale
at (703) 632-gg09.
if
applicable,
The submitted evidence was returned under separate cover

of communication.
Marc A. LeBeau, PhD

Chemistry Unit
(703) 632-7408
Technically reviewed and any identifications and associations

confirmed bv:
This report contains the opinions/interpretations of the examiner(s)

who issued the report.
Page 3
of3
070201013 PM GH
&.++,-
/5r\
7-251 (7-13-e8)
LABORATORY DIVISION
SUPPORTING DOCUMENTATION ENVELOPE
Case ID/ Sub
LzD-,/uW
qV ?1,3
IA Serial #
lor I
Please
Print Clearly
LtT3e*n
The Enclosed material for
supports LaboratorY RePort

Case ID, Sub and Serial
Name
11 O-z'o |
LabNumber(s)
013
Or WO Number
DescriptionofEnclosures itl
)'rv'n
Nole
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Chain of Custody
Communication and ActivitY Log
Notes
,{ {po't- {izes '

F ssL b,J,^- * b I
P
hsh'
I /''f"E
Pn
r,rs
Instrument Prrnt Outs, Charts, Graphs

Negatives
Photographs
ECS Search Slip
Shipping Invoice
please Return This Ilnvelope And
All contents To The
a
7-.lJBEr'io 0-06)
r^rl ni.û---.-,
Y,-Lg.
Hrui
FBI
2501 Investigation Parkway
Laboratory
Quantico, Virginia 221 35
REPORT OF EXAMINATION
Date: February 26,2007
Milwaukee
Squad 6/GBRA
SA Gerald E. Mullen
Case ID
No.: 62D-MW'443$-(ol
Lab No.: 070201013

Reference:
Communication dated January 30, 2007
Your No.:
Title:
STEVEN AVERY;
TERESA HALBACH-VICTM (DECEASED)
DOMESTIC COOPERATION -HOMICIDE
February 1,2007 and February 6,2007
The following items were examined in the Chemistry
Unit:
Q46
Swab (Item 9569)
Q47
Swab (Item 9574)
Q48
Swab (Item 9572)
Q49
Liquid blood sample from STEVEN AVERY (Item 9803)
K2
K3
Two control swabs Qtem 9801)
K4
This report contains the results of the chemistry examinations.
Page 1 of3
For Offrcial Use Only
6o ++t
( ss)
PM GH
Results of Examinations:
specimens Q46-Q49 and K2-K4 were
analyzed for the presence of ethylenediaminetetraacetic acid @DTA).
specimen Q49 was listed as a liquid blood

sample from sTEVEN AvERy in a
10
milliliter (mL) lavender-top blood tube. It contained
uppro*i*utely 5.5 mL of blood. EDTA was
identified in specimen
e49.
Specimens Q46-Q4s were reported to
be collection swabs of blood stains from
the
crime scene associated with the death of TERESA
IIALBACH. Specimen, rz-r+ were reported
to be control swabs collected in relation tg
.wabs. EDTA, either as the free acid or
s. Q46-Q4g
as the EDTA-iron cornplex, was not
identified
trr. q+o_e4g or K2-K4 swabs.
The analysis for EDTA was.carri.ed out using

liquid chromatography/tandem mass
spectromety in both positive and negative elechosprayfonization
modes.
Remarks:
EDTA is an,anti-coagulant and enzyme inhibitor

that is commonly used in blood
collection tubes' Blood specimen collection
tubes containing EDTA have lavender-colored
tops
and are the most common collection tube
used to collect refeience specimens for DNA
testing.
The concentration of EDTA in its free acid fonn
in a drawn blood tube is typically
1000-2000 milligrams per liter (mg/L), depending
on the uolu*, of blood and the capacity
of the
tube' At this concentation, the free acid and saliforms
of EDTA are soluble in blood. EDTA
readily forms water-soluble chelates with nearly
including iron in blood.
Aqueous extactions of dried bloodstains allowfor
the isolation of EDTA (both as the free acid
and as the EDTA-iron complex) ifpresent.
alldt;etals,
Using the procedurl.e.mnlg-red in this case, EDTA

is readily identified at a
concenbation of 13 mglL. Additionally, EDTA
is also detectable when 4
a r-'uvr'
l-microliter drop of
EDTA-preserved blood is
analyzed.
For questions about the content of this report, please

contact
at (703) 632-7408.
Page 2 of 3
070201013 PM GH
For Official Use Only
f, ++t"
( s'i)
unit chief Marc
LeBeau
For questions about the status of remaining

forensic
-i'' examinations,
please contact Request coordinator
Michael vanarsiare
if applicable,
rloz>632-gg09.
The submitted evidence was returned

under separate cover of communication.
Marc A. LeBeau, phD

Chemisty Unit
(703) 632-7408
Technically reviewed and any identifications

and associations confirmed by:
Date:
This report contains the opinions/interpretations

of the examiner(s) who issued the report.
Page 3
of3
070201013 PM GH
fn
vqb
(cr,\
7-25{ (7-13-98)
LABORATORY DIVISION
SUPPORTING DOCUMENTATION ENVELOPE
Case ID/ Sub
(,zD-/uW-aV?A3
lA
Serial #
orl
Please
Print Clearly
Lr&et'u
The Enclosed material for
supports Laboratory RePort

Case ID, Sub and Serial
Name
LabNumber(s)
01 tSt'o I 0 13
Or WO Number
. tl
Description of Enclosures
\ )rnqin
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P
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'de .- l7
Communication and ActivitY Log

Notes
Na
{po'l- 9i zccl
F ssL b,d"- -
Chain of Custody
6l
Instrument Print Outs, Charts, Graphs
Pnrcs
Negatives
Photographs
ECS Search Slip
Shipping Invoice
Please Return This Envelope And
All Contents To The
(Rcv. 0l-3
l'2003)
FEDERAL BUREAU
Precedeace:
To
DEAD]TINE
B I 09 / 2007
s Laborat,ory
oF tI{rtEsTlGATlOIU
DaEe: orl3 o/2007
Attn: Scientific Analysis Section
Chemistry Unit
Mark Lebeau
Fron:
Milwaukee
Squad 6/GBRA
r
,^^^\
Coatact,:SAGeraldE'MuIlen,(920)432-3868
APProved B-yr Greco RaYmond A
Drafted By: Mullen Gerald E:d1g
070201013
(Pending)-5b
Cage ID #: 62D-MW-44363
Tit,Ie:
STEVEN AVERY i
TERESA I{ALBACH-VICTIM (DECEASED)
DOMESTIC COOPERATION-HOMI CIDE
Slraopeie:Summaryo{captioned'matterwithrequestfor
aPProPriate examination'
Fg-
PackageCoPy:Beingforwardedunderseparatecoveraretrhe
following iEemst
To 3e Srlr.#q#
it,'1'c^rDt? blood'1) one box conta'ining vial human
fut,,':J'o
2) envelopes containing swabs from crime scene
tro(oziulto
was reported missing by family members
DetaiLs: Teresa Halbachrasr
seln on 10/3r/2005 on the property
ii7o3 /2oot. sn. was
yard with his family' Halbach
""
of steven Avery "n" "t""ofaasalvagg
vehiEle that was for sale as she
wa' Eaking pirotogiipit"
Numerous search warrants
worked for the Auto'Trader: magazine'and.
significant evidence was
were executed on the Averlr property
Alrery_1n the murder of Teresa
,""o.r"r"d implic"iing Steireir
--*tty
Sfreriff , 'Jerry Pagel' has requested
Halbach. The Cal;;;i
the assistance of the FBI fbr laboratory examinations.
stevenAverlgwasreleasedfromprisonin2003after
by DNA evidence' A vial
being exonerated for I rape conviction
drawn and, ueld to exonerate him in
of Avery,s Uf ooe, which wls
at the Manitowoc County Clerk
the rape conviction, was maintained
defense has aLleged the-investigators
of Courts Office. Avery'ssheriff's
Department used this vial of
county
from the Manitowoc
the crime scene implicating Avery in
blood to plant evidence lrc This
vial of blood contains EDTA'
murder of teresa Halbach.
RE;rURI.{ E\TIDENCP
ro lGirv nu Ys;-DIvIsloN
a-,/ q4b
4tltu/
To: Laboratory From: Milwaukee

Re: 62D-MW-44363 , 0L/30/ZOOI
The purpose of this reguest is to estabrish the
of EDTA, in the vial of -blood, thereby eliminating
the
allegation that this vial was used. t,o plant evidence.
Averyrs trial is scheduled !o began on o2/os/zool.
special Prosecut,or calumet county District
Attorney'Ken Kratz,
has -requested rhis examinaEion bi complered by oilbg/io07 ro
be
used ag rebuttal evidence.
presence
2
cf)
C-^/
(Vr-
fuz)
4/,w
-c)
N
O
f.-
To:
Re:
LEAD
I-,,aboratory From: Milwaukee

62D-MW-44363, Ot/30/2007
(g)
Set Lead, 1: (Action)

I,ABORATORY
AT OUANTICO, VA
Unit conduct appropriate examination of vial

of blood to determine the presence of EDTA. Conduct relevant
comparisons to swabs from crime scene. Conduct degradation
Tt is requested t,his examination be
anaiydis
-ompietedofbyblood.
03/Og/2007. The point, of contact from the Wisconsin
Oepirt,ment ;f .Tustice is Assistant Attorney General Norm Gahn at
Chemstry
(920) 418-4087.
ti
RETURN] EVIDENCE
TO MIL\TAUIiLE DiVISIO}tr
(Y)
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FBI Laboratory
7-243 (Rev.3-3r-04)
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Chain-of-Custody Log
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ID
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FBI Laboratory
Activity and Communication Log
Laboratory No.:
0nOA,Ol O t e,
Date
Case
ID No.:
D-Mw -*Vib.
Activity/Communication and Outcome
L/J/-q
By:
CO.(.
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Violation{s):
Lab No:
rstic Police Cooperation
070201013 PM
GH
City: Milwaukee, Wisconsin
Agency:
FBI
Form: Electronic Communication, 01/30/2007
Violation date:
Violation Location:
CaselD:
62D-MW44363
Seriat: 30
Latent Number:
Contributor No: 62D-MW-44363

Victim:
Subiect:
HALBACH, TERESA
AVERY, STEVEN
Cross Reference:
Remarks:
ECC Delivered to Unit:
Previous Submission(s)
o6t2270L2 PM Pv
Milwaukee, Wisconsin
FtsI
Electlonic
Qs:15-tl5
^-r 11{005
CoE'!. : t2/19 /2006

Ks
PM
NE IteE!:
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lraukee, Wisconsin
-4ectronic
Coua.
Ll/
01
/ 2006
Qs:13-1tl
06u08009
PM
Pv
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Electronic
Co&a.. :
tl/02/2006
Qs:11-12
060118254
Qc
Electronic
Conln. : Ol/
04/2006 ELna]-:04/
Qs:3-10
LL/2OO6
NE Jtahe:l
051123009 PM MR
l'lilwaukee, Wisconain
EBT
Electlonic
Co@,.
tl/L6/2005
Qs:1-2
el Method and No: Federal Express .7190 4673 4441

xes - l Date Received: 0210112007 -More
Received in ECC: 0?0il2007
0210712007 12:03:28 PM . mvanarsdale
fo 4+,
(
tr)
/vw
'
?-lzbln
ECU- I (Rev.7f27D005)
Evidence Control Unit

Evidence Check-In Notes
Laboratory Number: 070201013
PM
Case
ID: 62D-MW_44363
Received via FedEx one sealed box, tracking number 7lg0 4673 444l,containing:
one sealed box containing:
six sealed paper bags:
bag labeled "9569" contained:
one sealed envelope containing:
Q46 Swab (Item 9569)
bag labeled " 957 4' contained:
Q47 Swab (ltem 9574)
Q48 Swab (ltem9572)
one unsealed envelope containing: *envelope sealed in ECU*
one unsealed box containing: *box sealed in ECU*
NE2
Two control swabs (ltem 9801)

one unsealed box containing: +box seak:d in ECU*
NE3 Two control swabs (Item 9802)
one unsealed box containing: *box sealed in ECU*
NE4 Two control swabs (Item 9800)
a +q-b
Z-r)
/vw
ECU
- I (Rev.7/27D005)
Evidence Control Unit

Evidence Check-ln Notes
Laboratory Number: 070201013 PM
* indicates
Case
ID: 62D-MW-44363
unopened in ECU to preserve examinations, descriptions taken from packaginglEC
Received one sealed FedEx box TRK# 7190 4673 5091 (discarded in ECU) containing one sealed
box containing one sealed container containing one closed vial containing one purple top tube of liquid
blood:
Liquid blood sample from STEVEN AVERY (Item 9g03)
Q49
Initials of Preparer,&
Date: 717
u
Paee
fu+ut-
(tt)
l0+
1of-p
L.- Ln
4fi,\,
7-2 (Rev. 7-10-06)
Federal Bureau of Investigation

Laboratory Division
LABORATORY WORK SHEET
To: Milwaukee
Date: February 1,2007
Squad 6/GBRA
SA Gerald E.
Mullen
case rD
No.: 62D-Mw-44363
LabNo.: 070201013 PM
Reference: Communication dated January 30, 2007
YourNo.:
ritle:
STEVEN AVERY;
TERESA HALBACH-VICTIM PECEASED)
DOMESTIC COOPERATION.HOMICIDE
February t,2007
Specimens:
Q46
Swab (Item 9569)
Q47
Swab (Item 9574)
Q48
Swab Stem9572)
K: -NEZ-'['
.<'n
Two control swabs (Item 98,01)
$83-'l'
Kq NB+IF
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GENERAL DESCRIPTION OF EVIDENCE AND CONTAINERS (continued):
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02/0st2007
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070201013
02t05t2007
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Evidence Check-In $heet
Check-ln Dats:
OLlo0 lToo-J
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ID
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02/08/2007
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(l
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10
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('it)
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?;t,hre ESr
,M/o/e
TANDEM MASS SPECTRA

POS ESI MODE
Diagnostic lons (m/z)
response
ion ratio
pass / fail
m/z 132 247

91367.6 13928 7492.5
100.0 15.2 8.2
67724.8 9790.4 6929.4
100.0 14.5 10.2
PASS PASS PASS
response
ion ratio
pass / fail
m/z
91367.6
100.0
4349.5
100.0
PASS
160
Pos GontrolB
/,f
160
Pos GontrolA
Q49 LOD -
lul
132
15.2
0
0.0
FAIL
13928
247
7492.5
8.2
1803.5
41.5
FAIL
/-l
t.J'
m/z 132
91367.6 13928
100.0 15.2
150
Pos GontrolA
Q49 LOD - 2uL
response
ion ratio
pass / fail
1807.7
100.0
PASS
18.3
PASS
247
7492.5
8.2
2yha
698.7
7.1
PASS
fta4ar"rnls
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C:\Xcalibuirdata\Brewer\070201 013\21 623

RT:0.89
S#:66
M:837425
02116107 M:Q2:32
NL:1.25E5
fit/z= 159.S160.5
F: + c ESI Full ms2
+ c ESI Full ms2 293.00@1S.OO
293.00@15.001
12s.00-315.001 Ms
21623
Pos. Cont. A (MAL EDTA ext.)
21623#60-70 Rr: 0.81-0.95 Av: 11

F: + c ESI FuLI ros2 293.00015.00 f 1r<
Intensity
Relative
r32 .07
122 nt
I ?? qa
f J6.9b
160.04
160.80
t7
.64
zzz.6z
247 .L4
249.00
293.24
SilA 70
10(
9{
AA:77063
280.5
I3928.0
549.3
244.9
0.31
15.24
0.71
0.21
91367.5 100. 00
0.1 0.00
253.4 0.28
955.5 1.05
'709.4 0.?8
r92.3 0 .27
492.5 I .20
985.0 1. 08
3323. ? 3. 54
7
ffilz= 246.5-247 .5
F: + c ESI Full ms2
293.00@1s.00 I
125.00-315.001 MS
zlozJ
9(
T5
70
o
o
=a
o
: 2.08E5
Tlc
Ms21623
"t,lzt,lo:-
{,v +Vt
a'-
0l ozol o l3
C:U(catibur\'data\Brewer\07020
1 O1
OZ16107 04:35:06
RT:0.92
NL: 9.69E4
S#:68
n/z=
AA:535858
100-t
3U1 626
'1
59.5-1 60.5
F: + c ESI Full ms2

293.00@15.00 t
1 25.00-31 5.00t'MS
ztoz6
"u_1
+ c ESt Fuil ms2 293.00@15.00

I
Pos. Cont. B (Q49 ext.)
21625#63-7I RT: 0. B5-0.9G Av:9
F: + c ESJ Full rns2 293.00@15.00 I r25 . ..

Intensity
Relative
12' n
'
9790.4 14.46
1
l qa
"o
L60 .02
?)7
Cn
230.95
)'1A a)
246.93
z03.y5
214 .80
275.48
)oa )e
986.1
413.8
442.9
1.46
0.61
0.4
965.3
0.00
1.43
0. 65
57724.8 I00 . oo
1a?1 1
1213.l.
1. ?9
11
6929.4 la.23
27!.3
1631.9
499.9
2089.4
0.40
2.4L
0. ?{
3.09
S#:64
AA:51139
RT: 0.65
S#:4E
AA:,28/'O
NL:2.18E5
Ms 21626
Tlc
zl'o[ot
[* ++u
C:t(calibur\data\Brewer\070201
O1
3\2
RT:0.89
S#:65
629
0?/16107 05:07:38
.ii-sii,rrmsi'ziiioit6rf ,ioirii;ioo'jislSq
NL:4.34E3
trYz= 159.5-,160.5
1Oo_
F:+c551PrU."t
AA: 19603
?!3:3381333r"'
160
Spot LOD, 1uL e49
2152e#54_6s
P:.
@
+ 6 951 Fult
rns2
293.00@15.00
159.95
4349. q r no
n/z
Intensity
?19'?s
21629
293.33
Relative
t2S
^^
i;,ii:; ';;:;;
3758.0 85.40
. I tlE2
'10(
S#: &l
M:2958
9:
9C
80
75
70
c
o
o
NL:2.10E5
Ms 21629
Trc
&
qq-L
ll
tlvu [01
C:Xcalibur\data\BreweA070201
RT:0.9'l
S#:67
AA: 39228
01 3U 1 632
02116107 05:40:13
NL:9.04E3
+cESl
n/z= 159.5-160.5
F: + c ESI Fult ms2
?!3:33.9133&r"'
ms2 293.00@15.00
tZS.oo-Sts.oO1
Spot LOD,2 uL Q49
L632#65-6't Rr: 0. 88-0.91 ttF: + c ESI FulI ns2 293.00G15.00 L25 . ..

I
m/ z
Intensity
Relative
L32
21632
.64
160.01
fo/.uu
200.30
z90.Jb
250.08
?q?
11
1807.7 18.32
.3 32.11
9865.0 100.00
3227
758.7 1.69
1044.3
10. 59
598.? 7.08
2064.3 20.93
5131.0 52. 15
S#:47
1
00-l
AA:5E91
ru-J
ro-]
ru]
'l
'l
tuJ
-l
,A
65-l
.=
rrQ?
$\lfl /\t\P,
NL:1.68E5
Ttc Ms 21632
s vub
-ulr,"lol
Instrument Method:
EDTA
pos Swabs.meth
LCQ
Instrument Method
Creator: Administrator
Last. modifiedt 2/!6/07 by Administrator

MS Run
Time (min) : 10. 00
Divert, Valve: Dot used durinq run

MS
Detector Settinqs:
l- fnformation
Duration (min) : 10. O0
Number of Scan Events:
Segment
l_
Tune Method: EDTA_Pos_CfD

Scan Event Details:
1:
(293.0)->o(L2!;.0-315.0)
MS/MS: CE 15. O? ttsow 1.0
Pos
Friday, February 16, 2OO7 05:07203
t, 44b
z;
Page L of 2
QlaYcr a | 3
Or/rc lLco'J
Inst.rument,
Method: EDTA Pos Swabs . meth

Waters 2690 LC Svstem
Injector parameters:
Syringe draw rate (pI/sec):2.50
Injection vol-ume (p1) :5
Pump
settings:
Solvent A:5:95 ACN:Water + 0.06t

Solvent B:B
Solvent C:C
Solvent D: D
Min pressure (PSI):0
Max
NH4OH
pressure (PSI) :5000

nrr{- nrl{*-.. Dr
- -essure
frha rl-
Cha
rf
nrrf nrrf . Nnry1g]
Gradient program:
Time(min) Flow(m]/min) A(E) B(t)

0.00
0.30
100.0 0.0
3 .00
0. 30
100. 0 0. 0
C(S)
0.0
0.0
D(t)
0.0
0. 0
Curve
Llnear Li_near -
G
G
Timed events:
Initial states:
Switch L:No change
. Switch 2:No change
Switch 3:No change
Switch 4:No chanqe
(min)
0.00
firne
Event
Switchl
'
Action
No chanqe
Friday, February 15, 2007 C)5 : 07 ; 03
Parameter
/^
q'/
Page 2 of 2
c'1aL,r I cl3
crrfrr"ltc-'1
Seq uenc e---07 0201

Sample Name:
0 1 3_Pos.
sld [Open]
Dl H2O ext.)
(neg
C.,mment:
Study:
Client:
Laboratory:
Company:
Phone:

Unknown
Sample lD
21601
Path
C
Inst Method
Xcali bur\Data\B rewer\07 0201 0 1 3
Position
InjVol
5.0
Level
U:\ calrbur\methods\EDTA Pos Swabs
Sample
Wt
0.000
lSample
0.000
Vol
ISTD Amt
0.000
Sample Name: Neg. Control(-EDTA blood swab ext.)

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
unKnown
21602
02
C:
Proc
Cal File
Position
InjVol
5.0
Inst Method
U(calibu r\Data\Brewer\07 020 1 01 3 C:Xcalibur\methods\EDTA pos-Swabs
Level
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
/1/w
o7ola I o l3
f* v+,page
czf rr lz-o1
-l-tP
Sequenc e---070201 01 3_Pos. sld [Open]

Sample Name: BLANK (neg blood, Dl H2O ext.)
C^-rment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
21603
01
C:Xcal
Proc Method
CalFile
Position
1
njVol
Inst Method
ibu
r\Data\Brewer\07 020 1 0 1 3 C:Xcalibur\methods\EDTA pos Swabs

Level
5.0
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
t***t************************************t
Sample Name:
_r-l
Comment
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
lnst Method
UNKNOWN
21604
01
C:U(calibur\Data\BreweA07020
Proc Method
CalFile
Position
InjVol
Level
5.0
t**********************
t3 C:Xcalibur\methods\EDTA pos SteG
Sample Wt
Sample Vol
0.000
0.u00
STD Amt
0.000
**t*******t***t******************************+i******a*****
q(u
t"( r"")
oaoe2
a1c'tat ol3
orf rt,f Lool
-ir$
Seq uenc e--07 020

Sample Name:
3-Pos. sld [Open]
extract
Study:
C^rment:
Client:
Laboratory:
Company:
Phone:

Unknown
21605
Proc Method iCal File
lnst Method
Samole lD
Path
03
C:\)(calibur\Data\Brewer\070201
Position
InjVol
5.0
Level
013
C:Xcalibur\methods\EDTA Pos-Swabs
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
Sample Name:IBLANK (neg blood, Dl H2O ext.)

Study:
Comment:
Client:
l-aboratory:
r0ompany:
Phone:
Sample Type
ile Name
Samole lD
Path
lnst Method
tXcatiOu rtData\Brewer\07020
Unknown
21606
01
Proc Method
Cal File
Position
InjVol
5.0
Level
10 1
3 C:U(cal i bu r\methods\E
Sample Wt
Sample Vol
0.000
0.000
DTA-Pos-Swabs
ISTD Amt
]o.ooo
****************t***************t***t***i*********t*****
/"AA/.,p
{+
qvL,
(/or)
oaoe 3
c1o'Lc'lol3
o.tlrUltu,'1
JDR
Sequence--07 0201 0 1 3_Pos. sld [Open]

Sample Name:
C^"nment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
21607
01
Proc Method
CalFile
Position
InjVol
5.0
lnst Method
:\XcalibuAData\B rewer\07 0201 0 1 3 C:U(calibur\methods\EDTA
Level
Pos Swabs
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
t***t****s*tt********t*i**i***********************tft
Sample Name:
extract
Comment:
Study:
Client:
Laboratory:
llompany:
Phone:
Sample Type File

unKnown
Proc Method
21
Name
608
lCalFile
Sample lD
Path
04
C: \Xcal ibu
lPosition
14
InjVol
lnst Method
i\Data\Brewer\07 0201 0 1 3 C:Xcalibur\methods\EDTA
Level
5.0
Pos Swabs
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
t*****************************************f****************************t*i*******t************************************t
01o'La 1 o l3
fu
q(b
(t,r)
nanc 4
ozlrt,iu.,,7
Tttl
Sequence---07 020 1 0 1 3_Pos.sld [Open]

C-
-ment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
21609
01
Proc Method
Cal File
Position
InjVol
5.0
Inst Method
:XcalibuAData\Brewer\07020
Level
C:U(calibur\methods\EDTA Pos Swabs
Sample Wt
Sample Vol
ISTD Amt
U.OOU
0.000
0.000
Sample Name:
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
21610
01
Proc Method
Cal File
Posrtron
InjVol
5.0
nst Method
\Xca ibu AData\Brewer\07 0201 0 1 3 C:U(calibur\methods\EDTA

I
Level
Pos Swabs
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
*****tt********************t***t
ol
{*
qt/L,,
( t ol;
nane 5
a'Lo\ o13
c'lf tt l)-"--7
-rbF
Sequence---07 020
01
3_Pos.sld [Open]
Sample Name: K3 extract
C- -ment:
Study:
Client:
Laboratory:
Company:
Phone:
lnst Method
Sample lD
Path
Unknown
21611
05
C:Xcalibu r\Data\Brewer\070201
Proc Method
CalFile
Position
InjVol
5.0
Level
G:\XcaltDur\memo0s\tsu
Pos Swabs
Sample Wt
Sample Vol
ISTD Amt
0,000
U.UUU
U.UUU
**tt*********t*************
Sample Name: BLANK (neg blood, Dl H2O ext.

Study:
Comment:
Client:
Laboratory:
Company:
Phone:
Samole lD
Path
lnst Method
Unknown
21612
UI
C:U(calibu r\Data\BreweA070201
Proc Method
Cal File
Position
InjVol
5.0
Level
013
C:Xcalibur\methods\EDTA Pos Swabs
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
**i**********************
4/1/t'/
olo2-olol3
5r,V4r( r"v)
nenc
c,'r-
[ tt, I L.t
I_oF
c,l
Sequenc e---07 0201
01
3_Pos.sld [Open]
(^
.ment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
21613
01
Proc Method
CalFile
Position
InjVol
5.0
Inst Method
:XcalibuAData\Brewer\O70201
Level
C:XcalibuAmethods\EDTA Pos Swabs
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
*i******************t********************************t**ist**************t*t*t*t***ti**1************#**f,**t****t**
Sample Name: Q47 extract

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
21614
Proc Method
Cal File
Xcal
Position
lnjVol
5.0
bu AData\B rewer\O7 0201 0
Level
Sample Wt
Sample Vol
0.000
0.000
0.000
*********************
{* vvt
( rcs)
clola't t'r13
a'>ltt-lro"J
.r1rP
Seq uen c e---07 0201
0 1 3_Pos.
sld [Open]
Sample Name:
C- -ment:
Study:
Client:
Laboratory:
Company:
Phone:
Samole lD
Path
Unknown
21615
01
C:Xcalibur\Data\Brewer\070201
Proc Method
CalFile
Position
InjVol
5.0
lnst Method
Level
3 C:U(callbur\methods\EDTA
Pos Swabs
sample wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
Sample Name:
Comment
Study:
Client:
Laboratory:
Company:
Phone:

21616
Unknown
Proc Method tCal File
Sample lD
Path
01
Position
lnst Method
\Xcalibu r\Data\B rewer\07 0201 0 1 3 C:U(calibur\methods\EDTA
njVol
Sample
Level
Wt
rSample Vol
IST
0.000
0.000
Pos Swabs
0.000
5.0
t*********t****************************************************t***********l***********************l
O-7c>Lt t
fx a4rlrou\/
naoe
olf
ru
cl3
lz'"1
Tbp
Seq uenc e---07 0201 0 1 3_Pos. sld [O pen]

/^- -'rment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
21617
07
C:U(cal ibur\Data\Brewer\07020
Proc Method
Cal File
Position
lnjVol
5.0
Inst Method
Level
013
C:U(calibuAmethods\EDTA Pos Sw,bs
Samole Wt
Sample Vol
ISTD Amt
0.000
rJ.000
0.000
*t*******i*****************r******
(neg blood, Dl H2O ext.
Sample Name:
Comment:
Study:
,Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
21618
01
C :\Xca libu r\Data\Brewer\07 0201
Proc Method
Cal File
Position
lnjVol
5.0
Inst Method
Level
Sample Wt
Sample
0.000
0.00u
Vol
iISTD Amt
0.000
*****************************
5, qvL.
0lcLolol3
oLl lt
I z-"c 1
wF
Sequenc e---07 020
3_Pos. sld [Open]
C^-ment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
21619
01
C:U(calibur\Data\Brewer\070201
Proc Method
Cal File
Position
InjVol
5.0
Sample Name:
lnst Method
Level
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
extract
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Inst Method
Unknown
21620
08
Proc Method
Cal File
Position
InjVol
5.0
Level
013
lSample Wt
Sample Vol
0.000
0.000
STD Amt
10.000
******************t**************t
q+G
/o( t,s1
nana
1O
oJoLo\ o\3
6Ll \b I t-,'1
-TI'F
Sequenc e---07 020
3_Pos. sld [Open]
C^-rnent:
Study:
Client:
Laboratory:
Company:
Phone:
Samole lD
Path
Unknown
21621
01
Proc Method
CalFile
Position
InjVol
5.0
Inst Method
Level
3 C:D(calibuAmethods\EDTA Pos Swabs
Sample Wt
Sample Vol
ISTD Amt
U.UUU
0.000
U.UUU
*************

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
lnst Method
unKnown
21622
01
Proc Metnod
Cal File
Position
InjVol
evel
0't 3 C:XcalibuAmethods\EDTA Pos Swabs
lSample Wt
Samole Vol
Amt
5.0
U.UUU
0.000
0.000
f************
/*
,/'/ ('
(t"o)
oaoe
11
ol0Lol O l3
oLlit l2oc-i
T0fl
Sequenc e--070201 01 3_Pos. sld [OpenJ

Sample Name:
I
O^-rnent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Unknown
21623
09
Cal File
Position
InjVol
5.0
Proc Method
Path
:
lnst Method
\Xcallbur\Data\Brewer\07020
Level
U(ca libur\methods\E
DTA_poLSwaG
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
******t*********i*t*****t*****************************t*****t*****************
******************

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
ype File Name

Unknown
Proc Method
Sample lD
Path
21624
01
C:
Cal File
Position
InjVol
i1
Inst Method
\Xcalibur\Data\Brewer\O7 0201 01
Level
5.0
3 C : U(cal
bur\meth ods\E DTA_pos_Swa bs
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
************
F*********t*******************ft
{*
6
( tro)
L/4
naoe 12
************************
o-l
0LOl0l3
ui-ltClzooT
i-uP
Sequence--07020
Sample
tlame:
C^*rment
3_pos.sld [Open]
Study:
Client:
Laboratory:
Company:
Phone:
Darnpte
Unknown
01
21625
tu
lHam
Inst Method
:Xcalibur\Data\Brewer\0i0201
\ACat tDu
r\method s\EDTA_Pos_swa bs
**************************l**t********************************f******ft*i*******************t*************t*****************************i*******
Sample Name:
Cont. B (Q49 ext.)
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Samole lD
Path
Unknown
21626
10
C:DGalibur\Data\Brewe^0
Cal File
Position
InjVol
10
5.0
Method
lnst
Levet
]Sampte
u.000
Wt
Amt
lsampteTol
0.000
0.000
***tt********i************t**********i*********************************************
f*(r"\44a
nana
ol oLcl a l7
0Lll6l t-oa1
-r1rg
Sequence---07 020
3_Pos. sld [Open]
Sample Name:
C^rment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
21627
01
u: \xcattbur\Data\Brewen070201
Proc Method
Cal Fite
Position
lnjVol
5.0
Inst Method
Level
01
Xca
bu r\m ethod
s\EDTA_Pos_ Swabs
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
**************************s*****t*
************t******************

Comment:
Study:
Client:
l-aboratory:
Company:
Phone:
Sample lD
Path
Unknown
21628
01
Proc Method
Cal File
Position
InjVol
i1
Inst Method
:\Xcal ibu r\Data\Brewer\07 020 1 0 1 3 U:V\calrDur\methods\EDTA Pos Swabs
Level
5.0
Sample Wt
Samole Vol
ISTD Amt
0.000
0.000
0.000
{*(r ,L{a
t ,a)
oaoe 14
ol o Zo\0ll
oLllvl i,oc)
aoP
Sequenc e---07 020

Sample Name:
3_pos.std [Open]
LOD, 1uL
C^'nment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
21629
11
Proc Method
CalFile
iPositio1
InjVol
Inst Method
Level
b.0
3 u : v(cattb
r\methods\EDTA_pos_Swa bs
Sample Wt
Sample Vol
ISTD Amt
u.0u0
0.000
0.000
*************l*t*********t****t*******************************************t*tt**tf***********t********************t***********r****************
Sample Narne:
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Samole lD
Path
Unknown
21
01
C:\)(calibuirData\Brewer\070201
Proc Method
CalFile
Position
njVol
630
nst Method
Level
C:\)(calibur\methodstEDTA pos Swabs
Sample
0.000
i50
*************************
01
Wt
]Sampte Vol
0.000
ISTD Amt
0.
'*************************************************************************t********************
{u avu,
( tra)
oaoe 15
o1s7.o I c 1j
c:>ltulz,"
IV,F
Seq uenc e---07 0201 0 1 3_pos. std [OpenJ

Sample
'l t{ame:l
u^Tment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample Type Frle Name
Sample lD
Path
Unknown
21631
01
C:U(calibuAData\BreweJ\o2020
Proc Method
CalFile
Position
InjVol
5.0
Inst Method
Level
1O1
Sample
:U(calibu r\methods\EDTA_poi Swabs
Wt
lSampte Vol
ISTD Amt
0.000
0.000
0.000
***************t************************************t**t**t**t********ti*******************
Sample Name: Spot LOD,

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Proc Method
Cal File
Position
InjVol
12
5.0
Level
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
r**************t***************************************
/l,/r,U
{* uu,
(r,v\
naoe 16
61aL.. I all
cz{rr"f Laol
avP
Sequence---070201 01 3_Pos.sld [Open]

Sample Name: BLANK (neg
I H2O ext.)
C^-ment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample Type File
Name lSamole lD
Path
Inst Method
Unknown
21633
01
Proc Method
CalFile
Position
InjVol
5.0
:Xcal
bu
r\Data\Brewer\07020
Level
10 1
:l G:u(calibur\methods\EDTA pos Swabs
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
*****t*****t****t***************i********t*
f'u +rle'
(its)
oaoe 17
oloLol o13
ctzlrt lLo"-l
avF
Vial List---C. Xca li bu r\methods\brewer\07020 1 0 1 3\070 20 1 0 1 3

Position
Sample Type Level Sample lD
Pos. sld
Sample Name
Unknown
Unknown
02
Neg. Control (-EDTA blood swab ext.)
Unknown
03
K2 extract
Unknown
04
Q46 extract
Unknown
05
K3 extract
Unknown
06
Q47 extract
Unknown
07
K4 extract
Unknown
08
Q48 extract
Unknown
09
10
Unknown
10
Pos. Cont. B (Qa9 ext.)
11
Unknown
11
Spot LOD, 1uL Q49
12
Unknown
12
Spot LOD, 2 uL Q49
{o
++l-
(r,)
nana
QloLol al3
tlrc I loo.t
"
T\tP
TANDEM MASS SPECTRA

NEG ESI MODE

273 mlz
Z4t
Diagnostic lons (nVz)
100.0
response
ion ratio
pass / fail
7.9
43718.3 -1653
100.0
PASS
5.0
PASS
Pos ControlA
mlz
326
2413.5
100.0
PASS
8802
7.7
PASS
114448.8

273
m/z
23366
100.0
300
105085 W1
Pos Control
247
300
m/z
100.0
Q49 LOD - 1uL
response
ion ratio
pass / fail
3548.4
response
100.0
15.0
PASS
PASS
ion ratio
pass / fail
105085
100.0
8271
7.9

273 mlz
247

273 mlz
247
response
ion ratio
pass / fail
(,y
963.5
100.0
PASS
105085
100.0
12717.7
326
2413.5
10.3
531.7
10.3
8271
7
FAIL
m/z
23366
100.0
733.8
100.0
PASS
300
326
241t5
10.3
1561
212.7
FAIL
366
1q0.0
.9
4031
418.4
2413.5
10.3
01020 t o t)
4/W
,4+c,
/r,t\
zlrt,ln
C:rXcalibur\...\Negativelon\21635
RT:0.93 100.1
02116107 06:53:36
z"
z
M:22116
*J
41-49 RT: 0.78-0.93 AV: 3

c ESI SRU ns2 291.20e15.00
246.50-325.50
Intensity
Neg. Control GEDTA blood swab ext.)

RT:0.97
AA:47160
Relacrve
272.'t0
213.21
nr;l.lllilg-r
ev;
- c Esl SRM ns2 344.20G15.00 I 2

z- 298.00-326.50
z
Intensity
Relaltve
-z?s.
/(,//l,tn \
Mv /
\-/
o
o
D
f
o
o
Fr
299.70
98{.3 100.00
2153sil4?-sr
/(w
NL: 6.2085
illlz= 282.8-2U.3 F: - c
ESI SRM ms2
303.20@15.00 |
282.7*2U.251 MS
2't635
n
Time tminl
q"'N
ofi ?'oIo ,t)
( rtt)
Time (min)
C:Xcalibur\...\Negative lon\21 638
':l
RT:1.30 NL:1.36E3
M: 6867 Nz= 272.1273.5
02116107 07:26:12
F: -
ESI SRMms2
3il:339if
331
272.50-273.501 MS
z
246.8L
Intensity
K2 extract
z- 298.00-326-50
z
Intensity Relative
300.13
105?.3 LO0.0O
Relative
9{0. o 100. oo
tdz= 246.*217 .5 F: - c
ESI SRM ms2
291.20@15.00 [
246.50-217.fi.
272.50-273.501 MS
21638
I
6
I\t/'
nvz= 311.$312.5 F: - c
ESI SRM ms2
3s6.00@15.00 I
10(
311.5C.312.501 MS
21
638
4
I'
7C
55
50
45
40
to ,t:4b
(,r')
u'a,ln
Tlme (mrn)
C:U(cqllbuA...\Negative lon\2 1 641
rot
'l
aT. n ra
M:28309
02/16107 07:58:57
NL: 5.61 E3
Q46 extract
- c ESI sR!.{ ns2 344.20c15.00 [ 2

z- 298.00-326.S0
z
Inteosity Relative
299.'t9
2907. 0 1OO. 00
RT: 1.35
nlz= 272.5-273.5 F: - c
AA:18923
ESI SRM msz

291.20@15.00 [
246.50-247.fi,
272.sG273.501 MS
21il1
ttllL
^J\v
1
00-1
r/z=
^-l
ESI SRM ms2

356.00@15.00 I
311.5G312.501 MS
J--l
31 1.5-312.5 F: - c
21il1
--l
ol
Eo-l
7U
'-l
70i'
^-l
"l
60-l
JT
I
501
4s-l
I
oo-l
--l
^^l
*-j
d1llil
lW
f* r,q"
/ t ><t\
\?
Time (min)
C:\XcalibuA...\Negative lon\21 644
02116107
NL:0
r]iz= 272.5-273.5F: - c
ESI SRM ms2
291.20@15.00 [
1644#4I-49 RT: 0.78-0.93 AV: 3

- c ESI SRM ns2 291.20015.00
z- 246.50-326.50
contains no data.
08:31:35
K3 extract
RT: 1.20
AA: 6655
246.fi-247.fi,
NL: 1.75H!
mfz= 299.$300.5
ESI SRM ms2
216441f59-63 RT;
F:.
13333_9J333.r
272.50-273.501 MS
32s.5G320.501 MS
21644
1.12-r.20 ev:
- c ESI SRM ns2 344.20015.00 t 2

z- 298.00-326.50
Intensj.ty Relative
325.41
963.5 23.90
4031.0 100.00
NL:0
rnlz=246.5-247.5F: - c
ESI SRM msz
291.20@15.00 [
246.*-247.s.
272.5O-273.50j MS
I
E
{o
-E
RT;0.87
AA: 13:104346
NL: 1.24E6
nh= 242.8-2U.3
F:
.c
ESI SRM ms2
303.20@1s.o0l
282.75-2U.2q
MS
(Jq u
(ra,\
4ru\fl
C:D(calibuA...\Negative lon\21 647
02116107
09:04:15
Q47 extraci
;M:
RT: 1,81
AA:
NL:0
'n'lz= 272.5-273.5 F: - c
ESI SRM ms2
291.20@15.00 [
z=
246.50-326.50
conlarns no data.
z"
298.00-326.50
contains no data.
246.50-247.50,
272.50-273.50t MS
216/'7
RT:1.19
AA:4347
nlz= 2465-247.5 F: - c
ESI SRM ms2
rn/z= 325.t326.5 F: - c
ESt SRM ms2
I
I
l
I
291.20@15.001
246.50-247.50.
27?.fi-273.501 MS
u4.20@1s.001
299.5G300.5o,
g2s.s0-326.501 MS
21u7
I
I
"l
ol
6l
xl
tl
ot
<l
ol
6t
@i
-l
I
nlz= 282.8-2A43 F: - c
,ool
9H
303.20@1s.00 I
--l
21e47
rfz=
,5.1
242.75-2U.25l MS
on-l
NL:2.10E5
nn_
'-I
ESI SRM ms2
*l
.$,312.5 F: - c
iff:B&gllgr".
Il
'oJ
8q
qr--l
31
EStSRMms2
21u'|
solll
ll
'l,\
'u'l
'ol /lll
'l /l
'ol
ssJ il
I
_-l
*l
*-]
*l
*l
uo.lil
oul l\
oo'l I
orl
oo-l
*l
'u'l I \
I\
'o'l 1\
27
^^l
ar-l
2o-l |
lsll
Time (min)
6t,u,
/ t:>5\
'll\
'-1/
\
\
l.
ol-+-1->-+
Time (min)
"ili:
C:l(galibpr\...\Negative lon\2.1 650

RT:
':i
1.3A
M: 22883
0?/16107 09:36:53
NL:4.52E3
n,tz= ZTZ.+213.5 F: - c
ESI SRM ms2
K4 extracl
NLO
rn/z= 299.$300,5 F: . c
ESI SRM ms2
Scan contains no data,
3il:3391i33t
333:',39Jfi93t
272.50-273.501 Ms
325,5S.326.501 MS
216sO
rnlz= 246,5-247.5 F: - c
ESI SRM ms2
2s1.20@15.00 t
246.50-247.50.
272.so-223.50i Ms
21 650
rnlz= 325.5.326.5 F: . c
ESI SRM ms2
3/t420@15.00 t
-
299.50-300.50_
325.50-326.s01 MS
21650
@
o
@
l,w
lw
rvz= 311.$312.5 F: - c
ESI SRM ms2
3s6.00@15.00 t
31r5G312.501 Ms
r.4
t*
44b
( ral)
r,,0\o\J
0dils
C:U(calibur\...\Negative lon\21 653

NL:0
||r'z- 272.6273.5F. - c
ESI SRM ms2

291 .20@1s.00 I
246.50-247.50,
02116107 10:09:33
1-49 RT: 0.7?-0.92 AV: 3

c ESI SRM ns2 291.2015.00
246.50-326.50
conlains oo data.
Q48 extract
RT;1.04
NL:2.67E3
AA: 23310
rw2= 299.5-300.5 F: - c
ESI SRM ms2
t#3381333'
272.50-273.50t MS
325,50-326.50i MS
21653
nr, o. er-il?-iE-a- c ESI SRM ms2 344,20015.00 { 2
2I 653i|43-ss
F:
B,/zz
298 .00-326.
300.25
5O
Intensity
Relative
133.8 47,01
1561.0 100.00
NL: O
nJz= 246.5-247.5 F: - c
ESI SRM ms2
291.20@15.00 I
246.50-247.50,
272.sG273.s01 MS
21
653
o
o
d
@,
o
.g
o
=o
":44J,
NL: 8.53E5
mJz=
282.8-2&.3 F: - c
ESI SRM ms2

303.20@15.0O I
292.75-2U.25t MS
21653
^,afl:)
oo"^,'lo'r'
Cu-nt
( r"t+\
C:\XqglibuA...\Negative lon\21 656
02J16107 10:,42:14
2l656tt4s-49 RT: 0-85-0. 93 Av: 2

: - c ESI sRM ns2 291.20915.00
z=
246.50-326.50
t 2 ...

RT:0.97
AA:549785
Intensity
Relative
821t.0 1.81
344.20@15.00 [
299.50-300.50.
325.50-326.501 MS
21 656
r05085.0 100 ,00
AA: 90037
fflz= 246.1247.5
NL: 3.25E4
m/z= 299.5-300.5 F: - c
ESI SRM ms2
1656ia51-63
RT:0.9?-1.20 A1
- c ESI SR!.i ns2 344.20.a15-OO t 2

298.00-326.50
z
Intensity
Relative
z=
300.02
23366.0 100.00
ZCTJ.5
IU. JJ
F: - c
ESI SRM ms2

291 .20@15.00 [
246.50-247.50,
272.50-273.501 MS
21656
!oc
o
d
6
c.
Ay
Nz= 282.8-28/.3
F: - c
r/z=
31 1.$312.5 F: - c
ESI SRM msz
356.00@1s.00 t
ESI SRM ms2

303.20@15.00 I
282.7+2U.251 MS
/t/W
31'1.50-312.501 MS
21656
f"
'l-ime (minl
'.,ill
+*a
(,''ts)
Time (min)
C:U(qalihuA...\Negative
lon\21 659
l-1
RT:0.97
AA:2619370
100-.1
NL:2.28E5
m,2= 299.S300.5 F: . c
ESI SRM ms2
344.20@15.00 [
299.50-300.50,
325.50-326.501 MS
21659
- c ESI SRU nsz 344.20c15.00 I 2 ...

z- 298.00-326.50
z
Intensity
Rel.ative
299.91
114448.9 1 00. o0
326.04
8802.0 1.69
ESI SRM ms2
2s1.20@15.00 [
246.50-24?.50.
272.5G273.501 MS
21659
'-l
",1
8q
.o']
zN
'o']
65j
,. -|
@
^^l
.2 45-1
6
@
E 40l
?6J
*l
ro-]
24
,-l
ril
'-l
'l
roo-,
nr-l
*-l
M'
nlz=282.8-2U.3F:-c
/w
/1N^
NL:6.35E4
rnlz= 31 1.t312.5 F: - c
ESI SRM ms2
ESI SRM ms2

356.00@1s.00
30320@15.00 [
282.75-2U.251 MS
21659
311.50-312.50] MS
21659
ru-]
801
tA
^.]
ul
*-l
*-]
*-1
orl
oo-l
rrl
'"]
,.';,-i;
Q+u,
( ,'at'\
f ime (min)
C:U(qalibur\...\Negative lon\21 662

RT:0.85
1001 AA: 11851E
*l
02116107 11:47:36
Spot LOD, 1uL Q49

RT:0.88
AA:363506
nlz=272.5273.5F: - c
ESI SRM ms2
662f43-53 RTr O.g1-1.19 AV:6

- c ESI SRU ns2 344.20@15.00
298.00-325.50
29120@15
r5.00 [
246.50-247.50,
246.50-247
272.50-273.501 . MS
a
tooz
filz= 246.1247
.5 F: -
ESI SRM ms2
2s1.20@1s.00 [
246.50-247.fi.
272.50-273.501 MS
21662
o
o
45
o 40
(tw
/\1,,"
'NL:5.10E5
dz=
242.8-28,4.3F: - c
ESI SRM ms2
303.20@1s.oo I
282.75.2U.25t MS
21662
f* ++a
( r^z\
0.,';:L.
C:u(calibud...\Negativelon\21665
0?/17107 12:20:10
Spot LOD, 2 uL Q49
'
,.(
RT: 0.88
AA: 746703
m/a= 299.$300.5 F: - c
ESI SRM ms2
133:338J333t
325.sG326.501 MS
21665
nlz= 246.1247
- C-ESI SRM ns2 344.20015.00 [ 2

z- 298.00-326.50
z
Intensity Relative
286e?.s 100.00
3:: !9
r.o.z6
262.5
0.91
.5 F: - c
ESI SRM ms2

291.20@15.00 I
246.fi-247.50.
272.50-273.501 MS
21655
04
$,
00-l
*t
*-1
*i
4M
AI^"
@
o
F
7.04E4
rnlz= 282.4-2U.3 F: - c
ESI SRM ms2
r/z=
i3l7t9Jfi3t".
356.00@15.00 I
31 1.5-312.5 F: - c
ESI SRM ms2
3t'1 .50-312.501-MS
21665
Ail
ro-1
7l
,"1
*t
60-l
--
::l
'ul
45-1
rc-l
'-t
^^
'u-l
^ nrOl)
6: aa
( ,,s)
0'10',Jrr\*
C:'"'icalibur\data\Brewer\070201
01 3\2'l 601
Tfog
02116107 12:03:08
NL: 1.36E3
+ c ESI Full ms2 293.00@15.00 [ 125.00-315.001
rvz= 159.$'160.5
F: + c ESI Full ms2
'
293.00@15.00
12s.00-315.001 MS
2160'l
tnlT- 246.5-247.5
F: + c ESI Full ms2
293.00@1s.00 [
125.00-315.001 MS
21601
10
95
90
80
70
0
o
6
u
o
o
-g
66J--61
240
3.28
354
9.04
304 4.U
4.'15
cua
6zt
6.93 510 E.Ss
NL: 2.83E5
TtC MS 21601
nxnrnrT
05
cF
500
381
oll;l,a3'M{\',
C:)XcalibuAdata\Brewer\O7020
r,
t.
3\21 602
cDP
ozrcrc7
i2:14.29
NL:0
mrz= 159.5-160.5
F: + c ESI Full ms2
293.00@15.00 [
125.00-315.001 MS
160?#65 RT:o.EE AV: 1 NL: 7.25E3

: + c ESI Full ms2 293.00@15.00 [125.00-315.00]
21eo2
100-l
*l
nol
a nqEr
m/z= 246.5.247.5
F: + c ESI Full ms2
2s3.00@15.00 [
125.00-315.001 MS
21602
65t
.o-]
I
,o-l
I
ru-i
,q ^n-l
@
6u
('il)
41,/
C:VcalibuAdata\Brewer\O70201
O1
3U1 603
-rg
0?/16107 12:25:21
NL:
BLANK (neg btood, Dt H2O ext.)
JUJrcO A I : U.OO AV: 'I NL:
+ c ESt Fuil ms2 293.00@15.00 125.00-315.001

[
nvz= 159.$150.5
F: + c ESI Futl msz
293.00@15.001
i
25.oo-5i s.ool' Ms
21603
3.43E3
rnlz= 246.$247.5
F: +cESl Fullms2
293.00@1s.001
125.0G315.001 Ms
2l 603
o
o
E
o
.t onEE
Ttc
{\rs 21603
@
t"q K
C:Xcalibur\data\Brewer\07020
f\
Ol 3U 1 604
-lo6'
0A16107 12:36:16
:
BLANK (neg blood, Dt H2O ext.)
+ c ESI Full ms2 293.00@15.00 125.00-3iS.0OI

[
rnlz= 246.5-247 .5
F: + c ESI Full ms2
?33339f333rr^
o
o
o
.:
o
o
:1.1gEs
TIC i/ls21604
/1/y
ti+
/ta)
C$(calibur\data\Brewer\07020
\-
01
JDP
'
3U l 605
02116107 12:47:04
NL:0
K2 extract
+ c ESI Full ms2 293.00@15.00

[ 125.00-315.001
m/z= 159.5-160.5
F: + c ESt Full msz
293.00@15.00 |
125.00-315.00t MS
21605
ntlz= 246.5-247.5
F: +,: ESI Full ms2
293.00@15.00 [
125.00-315.00t Ms
21605
o
o
E
.z
-g!
NL: 9.45E4
Ms 21605
Ttc
7.U
@
Aw
5*
4+,
(rv\
C:\Xcalibur\data\Brewer\070201
rl
01 3121
606
-|vg'
0U16107 12:57:54
m/z= 159.5-'160.5
F: + c ESt Full ms2
293.00@1s.00 [
125.00-315.001 MS
21606
+ c ESI Full ms2 293.00@15.00

[ 123.00-315.001
: 2.81E3
100-l
ru-.1
ro-l
*l
ftlz= 246.5-247 .5
F: + c ESI Full ms2
293.00@1s.00 I
125.00-315.001 MS
21606
ro-l
to-]
I
--l
^^-.1
A/^/
C',Wcaliburtgata\Brewer\070201
01 3U1
607
DI'
02116107 01:08:5'l
NL:0
rn/z= 159.5-160.5
F: + c ESI Full ms2
293.00@15.001
125.00-315.001 Ms
: + c ESI Full ms2 293.00@1S.00 [ 125.00-315.00]
2',t607
m/z= 246.1247.5
F:+cESl Fullms2
293 00@15.00 [
125 00-315.001 MS
21607
@
^N
C:Uftalibur\datia\Brewer\070201
'l
0 l 3U1
60g
NL:0
rvz= 159.5-160.5
+ c ESI Full ms2 293.00@1S.00 125.00-315.001

[
F: + c ESI Full ms2

293.00@15.00 I
12s.00-51s.oot'Ms
21608
249
3.40
239
/vw
,L++
C:\XcalibuAdata\BreweA070201
01 3\21
609
nlz= 1 59.5-'160.5
F: + c ESI Futl ms2
;;Esr i;il
'U
2r!.bb61';:ddr
125.00-315.001
293.00@15.00 t
125.00-31 5.001'MS
21
609
'NL: 0
.r z=246.1247.s
r.,
F: + c 951 PrU
293.00@15.00 t
1 25.00-31 5.00t-Ms
21509
@
4/
,{r v

+ c ESI Full ms2 293.00@1s.00
[1z5.oo-315.00]
fre\
oy
Al,/
l{y
t1,
-C:U(calibur\data\Brewer\07020'l
01 3\21 6.1
t op
.l
o2t16to7 o1:52:18
NL;0
nvz= 159.5-160.5
rruJ
t. u.oo Av: I NL:
^ ms2 293.00@15.00
+ c ESI Full
[ i2S.O0-315.001
tr,
F: + c 551 Pu1,
293.00@15.00 [
125.00-315.001 MS
21611
100-l
ru-]
e0-j
e*]
.o-l
^-l
to-]
uuJ
^n-j
433
497
508
6.94
5.U
5.12
@
Al,/
ti+
C:U(calibur\datia\Brewer\070201
"--_ 0
3\2
ffip
oa$rc7
o2:03:10

Full ms2 293.00@1S 00 [ 125.00-315.00]
10(
oa
8C
/a
70
6
o
a
o
o
o
NL:3.196E5
425
Trc Ms21612
5.8't
^^^l
JOO I
@
A/N
t-uV
C:,\XcalibuAdata\BreweA07020't 013U1 6l 3

N!: o
nVz= 159.5-160.5
F: c ESI Full ms2
: + c ESI Full ms2 293.00@i5.OO
,|ZS.OO-atS.OOJ
293.00@15.00 I
125.00-315.00t MS
21615
mlz= 246.1247.5
00-l
F: + c ESI Full ms2

2e3 00@15.00 I
*-]
12500-315.001 Ms
*.1
uu-l
801
zs']
toJ
5s-l
I
i.ol -"-J
3ol
.9
4s-l
-^,1
40-.1
ro-]
ru-j
,ol
ru-l
ro-]
-l
702
@
^W
C:U(calibur\data\Brewer\070201
'i
O1
3U 1 61 4
drp
02116107 02:24:52
NL:0
+ c Est Futi
rn/z= 159.$160.5
F: + c ESI Fult ms2
,o? nn6la
^n
Q47 extract
mii 2s's.bb@idno"i
1z5.oo-31s.001
12s.00-315.001 Ms
21614
100
7.94E3
rnlz= 246.5-247.5
F: + c ESI Full ms2
90
ir,ifl3.sl833,r^
85
80
75
70
65.
o
o
o
NL: 3,86E5
Ttc t,ts 21614
@
I\IIP
- C :U(calibur\data\BreweA070201
\.,
3U 1 61 5
02116107 02:35:44
NL:0
rn/z= 159.$160.5
F: + c ESI Full ms2
,ol nnâ E nn I
12s_00-315.001 MS
216'15
oAlp
li,t,t
C:lKcalibuAdata\Brewer\070201
0 1
3U
61
frF
0?/16107 02:46:33
NL: 0
+ c ESI Full ms2 293.00@15.00 125.00-315.001

[
nvz= 159.5-160.5
F: + c ESI Full ms2
293.00@15.00 [
125.00.315.001 MS
t00
21616
1.70E3
tnlr-246.U247.5
F: +
c ESI Full ms2

2s3.00@15.00 [
12s.00-315.001 Ms
216'16
o
o
o
,:
.g!
.g
1.33E5
2'1616
Tlc lls
@
N,lv
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C:\)(calibur\data\Brewer\07020
0'l 3\21 61 7
02116107 02:57:25
01
NL:0
K4 extract
/fft5 r{t: 0.66 AV: I
NL: 5.63E3
+ c ESI Full ms2 293.00@ t5.00 125.00-315.00]

[
r/z-
159.5.160.5
F: + c ESI Full ms2
293.00@15.00 [
'125.00-315.001 Ms
21617
fiilz= 246.5-247.5
F: + c Egl Pu11
2e3.00@15.00 {
125.00-3'15.001 MS
t.,
2'1617
o
o
o
oa
o
.:
o
o
1.76E5
MS 21617
@
Aj,P'
tit +
rt
C:Vcalibur\data\Brewer\07020101
3\21618
:floyg
02t16t07 03:08:17
rn/z= 'l59.$.160.5
F: +cESl Fullms2
293.00@15.00 [
125.00.315.001 MS
21618
1001
ru-l
ro-1
ro-]
I
ru-l
70-J
--l
^.-l
"n_l
c ESI Full ms2 293.00@15.00 [ i25.o0-3i5.ool
C.:\Xcalibur\data\Brewer\070201
01 3U
161
fttF
o2t16tot o3:1e:12
NL:0
nvz= 159.5.160.5
F: + c ESI Full ms2

,ol nn6r a nn r
125.00-315.001 MS
; ; l-sl ini
'-ii
zg'g.bbtb
iiio'
r I 2s.00-3 I 5.00I
2't619
A AOEt
10(
rrlJz=246.5-247.5
F: + c ESI Futl ms2
?:33393#rr^
oa
80
70
o
o
of
o
-=
6
tr
Ttc
{./ /EC
Ms 21619
@
AtN
tr'/
C:\Xcalibur\data\Brewer\070201
3\21
fi4
620
tL
oz16to7 o3.29:s7
NL:0
nvz='159.$'160.5
F: + c ESI Full ms2
293.00@15.00 [
125.00-315.001 MS
21620
+ c ESI Full ms2 293.00@1S.00 125.00-315.001

[
laa
7.90
@,
/\Ilv
C:U(calibur\data\BreweA070201
3\21 621
T-ry
02116107 03:40:49
NL;0
+ c ESI Full ms2 293.00@1S.00 125.00-315.001

[
rvz= 159.5.160.5
F: + c ESI Full msa
!i!1{38r33&',.
: /./cEJ
rnlz= 246.9247 .5
F: + c ESI Full msz
293.00@15.00 [
125.00-315.001 MS
21621
1001
nl
rol
"-l
ro']
tul
to-l
6si
-^-l
o
o
6
.:
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flc
Ms21621
fl,^ 3ll
%
,{+ v
/t
C:D(calibur\data\BreweA070201
3U1 622
{n(t
02116107 03:51 :42
lttzzfttt t{t: u.66 Av: 1
NL:0
m/z= 159.$160.5
F: + c P51 Pr11
293.00@15.00 [
125.00-315.001 MS
NL: 1.13E4
: + c ESI Full ms2 293.00@15.00 [ 125.00-315.001
t.t
21622
Z.OJEJ
8.40
mh=246.5-247.5
F: + c ESI Full ms2
293.00@15.00 [
125.00.3'15.001 Ms
21622
54
o
5JZ
7.28
o
'a
o
o
38
36
NL:
rc
4.i'1E5
34
Ms21622
391
5.35
427
5.84
5'18
7.09
546
3.?2
209
z.w
20s
@
rus
C:U(calibuAdata\Brewer\07020
01 3\21
623
02116107 04:02:32
NL:1.33E5
+ c ESI Full ms2 293.00@15.00 [ 125.00-315.001
n/z= 159.5-160.5
F: + c ESI Full ms2
293.00@1s.00 [
125.00-315.001 MS
21623
o
o
6
o
o
Ttc
4.42
Ms 21623
419
475
5.72 6.49
,M
?oJ.hoL
\,$v
Lg-
Q:U(calibuddata\Brewer\070201
01 3U1
624
d"$
0U16107 04:13:22
324#65 Rr: O.E6 AV:
NL:0
+ c ESI Full ms2 293.00@15.00 [125.00-315.001
NL:0
nvz= 159.$160.5
F: + c ESI Full ms2
2s3.00@1s.00 [
12s.00-315.001 MS
21624
'NL: 6.06E3
nlz= 246.5-247 .5
F: + c ESI Full ms2
293.00@15.00 [
125.00-315.001 Ms
21624
100-l
"l
*t
^-l
6J
*t
qEl
80J
71)
.^l
^_l
ol
l
621
8
le
ees
.z
.g
NL:4.63E5
5.El
Ttc Ms21624
407 l4
4.0 s.56
lJ
/W
,/l
-i
C:Xcalibur\data\Brewer\07020
01 3U1
0?/16107 04,'24:14
625
1 NL: 2.9EE3
: + c ESI Full ms2 293.00@15.00 [ 125.00-315.00]
1625#5 RT:0.E6 AV:
rn/z= 159.5-160.5
F: + c ESI Full ms2
293.00@1s.oo I
125.00-315.001 MS
21625
4.54E3
246.5-247.5
F: + c ESI Full ms2
293.00@15.00 [
125.00-3'15.001 Ms
tlz=
21625
o
o
o
o
o-
4.97E5
Ttc
4.1
MS 2'1625
289
3.95
ssg
8.19
| 9.29
ll
@
}IM
4
/ t<,
teV
0U16107 04:35:06
+ c ESI Full ms2 293.00@15.00 [ 125.00-315.001

160
00-l
*t
rol
*l
"-l
75-l
-^l
--l
^:
C:XcalibuAdata\Brewer\070201
01 3\2
1626
()
"
u)
TbF
oa't6n7 o4:35:06

1
NL:1.08E5
rdz= 159.$160.5
+ c ESI Full ms2 293.00@15.00 [125.00-315.001
F: + c ESI Full ms2

293.00@15.00 [
125.00-315.001 MS
21626
fflz=246.5-247.5
F: + c ESI Full ms2
293.00@1s.00 [
125.00.315.001 MS
ztozo
@
A^jl'J
{"+
/;<
-ID$
0A16107 04:45:57
n/z= 159.$160.5
+ c ESI Full msz 293.00@ 1 5.00 [ 125.00-31 5.00]
F: + c ESI Full ms2

293.00@1s.00 [
12s.00-315.001 Ms
21621
NL:1.23E4
rnlz= 246.5-247.5
1001
F: + c ESI Full ms2

293.00@15.00 [
'125.00-315.001 MS
21627
s5-.1
*l
on-l
"-l
"n-l
;L
'-l
7o-l
I
--t
o --l
!
o
6
o.Jz
zsz
i6^3^
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7.24
646
8.84
624
8.54
Ttc
4.66E5
Ms 21627
|
I
ffN
Co+
C:Xcalibur\data\Brewer\O7020
01 3U
628
',w
02116107 04:56:49
NL:0
r/z=
+ c ESI Full ms2 293.00@15.00 125.00-315.00]

[
159.5-160.5
F: + c ESI Full ms2

2S3.00@15.00 I
125.00-315.00] MS
2162A
o
o
G
.:o
6
o
Tlc
Ms 21628
,{* q
/ i1'7
01 3U
629
OA16107 05:07:38
Spot LOD, 1uL Q49
+ c ESI Full ms2 293.00@15.00 125.00-315.001

[
NL: 5.73E3
r/z= 159.t160.5
F: + c ESI Full ms2
293.00@15.001
125.00-3r5.001 Ms
21629
rlz=246.1247.5
001
F: + c ESI Full ms2

293.00@1s.00 [
125.00-315.00] MS
21629
ss-J
ro-l
ru-l
:t
r
309
"-]
zo-l
4.03
651
o
o
-".1
po
o
,:
6
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5.46
4.50
3091
2.1
taq
i ros
|
NL: 5.1 6E5

Ttc t\,ts 21629
AA?
7.68
ô99
zJo
@
Atrr
:U(calibur\data\BreweA07020
01 3\21
Spot LOD, 1uL Q49
629
1629F64-O5 t{t: 0.6/{t.69 AV: Z NL: 4.35EJ

: + c ESI Full ms2 293.00@15.00 [ 125.00-315.00]
::r
4
*l
uo-]
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ro-1
65-l
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0.64
/'r
0.75
,rril'\/4
{+q
/t
<,
C:\jt(calibur\data\Brewer\070201
.
01 3U
630
-Jnp
02/16/07 05:'18:30
NL:2.02E3
+ c ESI Fuil ms2 293.00@15.00 125.00-315.00]

[
rvz= 159.$160.5
100-
F: + c ESI Full
*-]
z5J.W@ tC.UU
ms2
I
125.00-a15.OOl'MS
21630
: 7.1 1E3
n122246.1247.5
10c
F: + c ESI Full ms2

293 00@15.00 [
12500-315.001 MS
2't630
85
EC
r!
70
228
211 3.12
o
o
o
0a
o
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tr
@
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4..
00f
^-l
"-l
01
3Ul 631
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0A16107 05:29:22
NL: 1.42E3
nvz= 159.5-160.5
F: + c ESI Full ms2
293.00@15.00 I
031t65 RT:0.88 AV:
NL: 1.0384
+ c ESI Full ms2 293.00@15.00 125.00-315.00]

[
125.00-315.001 MS
21631
@
r1|\/
{u tt|
C:Xcalibur\data\BreweA070201
=---
01 3U1
f,DF
632
0U16107 05:40:13
IOJMO X I ; U.YU AV: 1 NL: g.Z/E3

F: + c ESI Full ms2 293.00@15.00 [ 125.00-31S.00]
67
NL: 1.27E4
0.91
rn/z:159.$160.5
'05
o<J
F: + c ESI Full ms2

293.00@15.00 [
125.00-315.001 MS
*t
ztoJz
:4,25E3
mlz=246.U247.5
1001
F: + c ESI Full ms2

293.00@15.001
125.00-315.001 MS
z toJz
'-l
oJ
*l
*-]
ro-l
tr-]
to-l
*i
'-l
orl
oo-1
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ro-l
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1
0-1
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461
618
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356
876
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01
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632 (2.:vâ
) ar\
0416107 05:40:13
r
NL:127E4
nvz= 159.$160.5
F: + c ESI Full ms2
2e3.00@15.00 [
125.00-315.00t MS
21632
NL: 3.51 E3
.r,lz=246.5-247,5
F: + c ESI Full ms2
293.00@15.00 [
125.00-315.001 MS
2'1632
o
o
f
o
6
o
2.30E5
21632
Trc Ms
fn
Spot LOD,2 uL Q49
oozrco n t ; u.vu Av: t
NL: 9.2/Eo
+ c ESI Full ms2 293.00@15.00 125.00-315.00]
[
C:\,Xcalibur\data\Brewer\O7020
01 3\21
633
l-s oF
02116107
05:5't:09
m/z= 159.!160.5
F: + c ESt Fult msz
293.00@15.001
125.00-315.001 Ms
21633
+ c ESI Full ms2 293.00@15.00 125.00-31S.OO]

[
1001
ro.l
,A
ot.L
*ll|l
^.ll
^ll
,ll
*ll
279
3.81
344
4.70
2U
@
AI\}.v
C:'XcalibuA...\Negative
lon\21634 A70Zol
t3
j-oF
02116107 06:42:35
NL:0
nlz= 272.5-273.5 F: - c
ESI SRM ms2
291.20@15.00 t
246.50-247.50.'
272.50-273.soi Ms
2163/
NL:4.52E3
trlz= 246.$247.5 F: - c
ESI SRM ms2

291.20@15.001
m/?= 325.5-326.5 F: - c
ESI SRM ms2
246.50-247.50.'
272.so-273.s0i Ms
2163/
133339J,133r
325.50-326.s01 MS
8
o
"E
o
@
nîL
nlz= 282.t1-284.3 F: - c
ESI SRM ms2
r/z=
lSiiS.gJfj$r",
ESI SRM ms2

356.00@15.00 I
31
31
1.5-3i2.5 F: - c
1,50.312.501'Ms
2163/.
C:\Xcalibu^...\Negative
100r
*l
-"1
--
lon!21635 070/.O I Ols
02116107 06:53:36
NL:2.68E3
nlz=272.5-273.5 F:. c
rn/z= 299.5-300.5 F: - c
ESI SRM ms2
344.20@15.00 I
ESI SRM ms2

29'1.20@15.00 [
246.50-247.50.
299.50-300.50.-
272.50-273.50i MS
21
Neg. Controt (-EDTA blood swab ext.)
325.50-326.501 MS
635
21635
/Tr'z=
246.1247.5 F: - c
ESI SRM ms2

291.20@1s.00 t
246.50-247.50,
272.50-273.s01 Ms
21 635
@
/\,P
100-l
*l
*.1
ntz= 282.8-28/..3 F: - c
ESI SRM ms2
303.20@t5.00 I
282.75-2U.251 MS
2'1635
85-J
'o-l
tu-l
1l
or-l
uo-J
*l
uo-]
AtIt/
ou-l
oo-]
ru-]
rol
ffi,v
ntuv
C:D(calibur\...\Negative lon\2 1 636
e7ozotol3
Jop
0?J16107 07:04:28
rvz:299.$300.5 F: - c
ESI SRM ms2

344.20@15.00 t
299.50-300.50.'
325.50-326.50i MS
toJo
%
tol
'l
no-J
ru-l
nlz=246.5-247.5 F: - c
rvz= 325.5-326.5 F: - c
ESI SRM msz
ESI SRM ms2
lil:33.91f 33t
272.s0-273.501 MS
3d3339J333r
21636
325.50-326.501 MS
80'j
zs-]
zo]
^-l
ol
scl
oo-]
rn/z= 282.8-2U.3 F: - c
ESI SRM nrsz
l3l?&gJfi3'r",
21636
ANW
f.vqa
C:Xcalibur\...\Negativelont21637
077LOlO13 J'lp
0?/16107 07:15:23
NL:0
flilz= 272.5-273.5 F: . c
ESI SRM mis2
291.20@15.00 l
246.50-247.50,
272.s0-273.501 MS
21637
1001
ssl
ro-l
ru'l
ro-l
"-l
,o1
*-1
60-l
8
d
o
-q
fitlz= 282.8-284.3F: - c
ESI SRM ms2

303.20@15.00 I
282.7s-2U.251 MS
ltoJt
oo-]
NL:4.16E3
s0-1
rn/z= 31 1.$,312.5 F: - c
ESI SRM ms2
356.00@15.00 I
31 1 .50.312.50t' MS
*l
es-]
Eo-]
ruJ
70J
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.o-]
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4s-..1
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^-l
"'-l
3q
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20i,
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ro-]
frt 4,/r.
/,,
C:D(calibur\...\Negative
,o5
e$l
lon!21638 A7 OLl
IoI
-tD p
0?16107 07:26:12
NL: 1.36E3
rnlz= 272.5-273.5 F: . c
ESI SRM ms2
291.20@15,00 [
246.50-247.50,
272.s0-273.501 MS
21638
4.04E3
ftlz= 246,5-247 .5 F: - c
ESI SRM ms2
291.20@15.00 [
nvz= 325.5-326.5 F: - c
ESI SRM ms2
344.20@15.00 [
299.50-300.50.
325.50-326.501 MS
21638
246.50-247.50,
272.50-273.s01 MS
2'1638
q
1001
nl
fflz= 282.&2U.3 F: - c
*-l
282.7r2U.251 MS
ESI SRM ms2

303.20@15.00 [
21638
:f
i:1
,"-l
'l
uo-]
--l
-^l
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ou-j
40-J
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30-l
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4(
8.73E4
m/z= 31 1.5-312.5 F: - c
ESI
SRM msz
3s6.00@ 1 5.00 [
311.50-312.501 MS
21638
Q:U<calibur\...\Negative
lon\21639 01A7Ol
0l
JTP
02116107 07:37:08
NL:0
rnlz= 272.5-273.5F: . c
ESI SRM msZ
291.20@'t5.00 |
246.50.247.50.
272.50.273.501 MS
21639
r lz=246.5-247.5F:-c
m/z= 325.5-326.5 F: - c
ESI SRM ms2
ESI SRM ms2

291.20@15.001
344.20@15.00
246.50-247.50,
299.50-300.50,
272.50-273.501 MS
325.50-326.501 MS
21639
21639
.E
@
4,ur'
Aw
001
--l
*-l
--t
*l
rr'z= 282.9-2U.3 F: - c
ESI SRM ms2
303.20@15.00 I
282.75-284.251 MS
21639
m/z= 311.5.312.5 F: . c
ESI SRM ms2
356.00@15.00 [
311.50-312.501 MS
21 639
80-l
__l
,
"-l
ro-j
rul
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*i
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C:\XcalibuA...\Negativeton\21640
C70Z0l0lJ
16p
0?J16t07 07:48:03
NL:0
tr]/z=272.5-273.5 F: - c
NL:9.94E3
n/z= 299.5-300.5 F: - c
ESI SRM ms2

291.20@15.001
246.50-247.50,
272.50-273.501 MS
21640
ESI SRM ms2
133339J333r
32150326.501 MS
m/z= 325.5-326.5 F:. c

ESI SRM msz
344.20@15.OO I
299.50-300.50,
325.50-326.501 MS
216/0
.p
n0t"
NL:0
nlz= 282.8-284.3
F:
ESI SRM ms2

303.20@15.00 [
2?21s-2u.2sl Ms
1.05E4
nVz= 31 1.t312.5 F: - c
ESI SRM ms2
356.00@15.001
311.s0-312.501 MS
21
640
At\lv
{*
aa
C:tXcalibur\...\Negative
| 001
95-..1
"l
ton\21641 0l0LOl
13
a6p
02116107 07:58:57
NL: 5.61 E3
rlp
272.5-273.5 Ft - c
ESI SRM ms2
291.20@15.00 [
246.50.247.50,
272.50-273.501 MS
21/1
100-.]
ru-l
rr'z= 246.5-247 .5 F: - c
ESI SRM ms2
291 .20@15.00 I
'o-l
*-l
246.50-247.50,
272.50-273.501 MS
216/.1
NL:5.66E3
nvz= 299.$300.5 F: - c
ESI SRM ms2
344.20@15.00 I
299.50-300.50.'
325.50-326.501 MS
21641
NL:2.19E3
n/z= 325.5-326.5 F
ESI SRM ms2
34420@15.00 [
299.50-300.50,
325s0-326.501 MS
ul
^K
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70-..1
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NL: 8.52E:5
fiilz=2828-2U.3F'. - c
ESI SRM ms2

303.20@15.00 I
282.75-2U.251 MS
^-l
o"-l
21/1
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,"1
"'l
^-l
60J
-*l
*l
45-1
oo-l
as-..1
r-l
I
A\1^',
C:\Xcatibur\...\Negativeton\21642
OlLLOl0lJ Jnl
0?/16107 08:09:50
rnlz= 272.5-273.5F: . c
ESI SRM ms2
291.20@15.00 [
246.50-247.50.
2z2.so-273.50i Ms
216p2
00-
'J
,ol
I
ru-l
m/z= 246.5-247.5F:. - c
ESI SRM ms2
291.20@15.00 I
trvz= 325.5-326.5 F: - c
ESI SRM ms2
344.20@15.001
299.50-5oo.so.'
325.50-326.501 MS
21d42
246.50-247.fi.
272.s0-223.50i Ms
21642
80-l
t*l
I
to-l
-l
eo-l
o
o
0nv
0J
1001
95i
*_l
rnlz= 282.5284.3 F: . c
ESI SRM ms2
303.20@15.00 [
282i5-2U.251 MS
*-l
so-l
ruJ
70!,
^-l
oc.o-]
I
s5-J
so-l
ou-l
oo-l
ru-1
"-l
5,r (4,
.g
@,
/r{
C:u(caliburl...\Negarive
lon\21643
0T0Zo/ot3 lTp
02116107 08:20:45
m/z= 299.5.300.5 F: - c
ESI SRM ms2
y4.2O@15.AO
I
299.50-300.50.'
325.s0.s26.50i MS
216/3
rtlz= 246.5-247.5 F: - c
ESI SRM ms2
291.20@15.00 [
246.fi-247.50,
272.50-273.501 MS
21643
r$/
s.89E3
nlz=282.8-2U.3'F:, - c
ESI SRM ms2
303.20@1s.00 [
282.7*2U.251 MS
21/.3
m/z= 325.5-326.5 F: - c
ESI SRM ms2
344.20@15.00 [
299.50-300.50.
325.50-326.501 MS
21/3
@
^N
C:lXcalibur\...\Negativeton\21644
0ZoZolo/3
JDB
0?/16107 08:31:35
Nz= 272.5-273.5F: -
K3 extract
rvz= 299.5-300.5 F: - c
ESI SRM ms2
ESI SRM ms2
ill:339ii33,t
133:33J333t
272.50-273.501 Ms
325-s0-326 501 MS
rrvz= 246.$247.5 F: - c
ESI SRM ms2
29120@15.00 I
246.50-247.50.-
zzz.so-zz:.soi
2'tu4
tr,ts
o
d
%
1.24E6
rdz= 282.t]-284.3 F: - c
:3!?39;figr".
o
@
*{}
%
1.09E5
rvz= 311.5-312.5 F: -
ESI SRM ms2

356.00@15.00 I
311.50.312.501 Ms
J\I},
,Y4
C:U(calibuA...\Negative ton\21645
01 0L0
i O 13
Tnp
0U16107 08:42:24
NL:0
mtz= 272.5-273.5 Fi - c
ESI SRM ms2
291.20@15.00 I
rn/z= 299.$300.5 F:
ESI SRM ms2
246.5G247.50.'
272.50.273.501 MS
!i3:338J'133t
216/5
!ffi-ezo.sot
us
, tot2
trlz= 246.*247.SF:. c
m/z= 325.5326.5 F: - c
ESI SRM ms2
344.20@15.00 t
299.50-300.50.325.50-326.501 Ms
216/.5
ESI SRM ms2

29',t.20@15.O01
246.50-247.50.-
272.50-273.50t MS
2't
645
o
o
E
@
AI.J
m/Sz=
282.&284.3 F: - c
;if,3.gJ."'3lr^
5y:4a
-c
o
o
nN
nVz=
311.$312.5 F: - c
ESI SRM ms2

356.00@15.00 I
311.50-312.501'MS
21645
C:Uftalibur\...\Negative
lon\21646 070LO t Ol3
frg
02116107 08:53:19
NL: 4.51 E3
100-l
I
J3l
."1
NF272.5-273.5Ft

NL:6.52E3
-c
rn/z= 299.5-300.5 F: - c
ESI SRM msz
ESI SRM ms2

291.20@15.00 [
344.20@1s,00 I
299.50-300.50.'
246.50-247.50.
272.50-273.501 MS
216/,6
32s.ss326.50i Ms
216/6
mlz= 246.5-247 ,5 F: - c
ESI SRM ms2
4.2'1E3
29120@rs.00 [
246.50-247.50,
272.50-273.501 MS
2't646
Io
r*/
10(
NL: 9.77E:3
mlz= 282.8-28/..3Fi - c
ESI SRM ms2
303.20@1s.00 [
282.75-2U.251 MS
21,!6
65
{o
F
@
Alt'"
nvz= 3'l1.5-312.5 F: . c
ESI SRM ms2
355.00@1s.00 I
311.s0-312.501 MS
21646
75
7A
65
OU
55
4n
45
40
30
z,t 4*b
Î\J'p
C:\Xcafibtlr\...\Negative lon\2,|647
Al|Lot
ol3 ftA
02J16107 09:04:15
NL:
Q47 extract
f,tlF 272.+273.5F: - c
ESI SRM ms2
291.20@1s.001
246.50-247.fi.
272.50-273.501 MS
21/7
rvz= 299.5.300.5 F: - c
ESI SRM ms2
344.20@1s.00 I
299.50-300.50,'
325.5G326.501 MS
21647
m'lz= 246.5-247 .5 F: - c
ESI SRM ms2
29120@1s.001
245.50-247.50,
272.50-273.501 MS
21647
flv
rniz= 325.t326.5 F: . c
ESI SRM ms2
344.20@15.00 [
299.50-300.50,
325.50-326.50t MS
21647
tv
C;iXcalibuA...\Negative
lon\21648 0702o/
Ot? ftp
02J16107 09:15:08
NL:0
rj/z=272.5-273.5F:
NL:0
-c
ESI SRM ms2

291 .20@15.00 r
rilz= 299.1300.5 F: - c
ESI SRM ms2

344.20@15.001
299.50-300.50.325.50.326.501 MS
246.s0-247.50.'
272.50-273.s0t Ms
216/.A
21&t8
1001
nu-J
*-l
'l
mE= 246.5-247.5
F..
-c
29120@15.00 t
246.so-247.s0.'
rvz= 325.5-326.5 F: . c
ESI SRM ms2
344.20@15.00 r
272.50-273.501 MS
299.50.300.s0.'
ESI SRM ms2
216/.8
325.s0-326.501 MS
21il8
ro-l
75-l
?o-l
6s-l
'l
oo-l
o
o
@
nN'
n,lz= 282.9-2U.3 Fi - c
ESI SRM ms2
303.20@1s.00 I
282.7U2U.251 MS
o
o
w
:
7.49E3
rvz=
31
1.S312.5 F: . c
ESI SRM ms2
356.00@15.001
31150-312.501 Ms
f'ftl,/
["
q'/
C:U(calibur\...\Negative
lonl21649 CI7oLol
OIZ 6g
0A16l07 09:26:04
NL:8.15E2
'iil
rrllz= 272.5-273.5 F: . c
ESI SRM msz
291.20@15.00 [
246.50-247.50.
272.50-273.501 MS
21.4.9
2.3183
1001
,5-l
e0-J
*-l
t.F Psiit*1f;L:'jt
|
t''"
291.20@15.00 r[
246.50-247.50,
27250-273.s01 MS
80-..1
t;
^]
6q
I *-]
t
a
nr/
rol
"-l
o^J
--l
^-l
""1
ro-1
trJ
1t
::r
o"l
*l
*l
qnJ
oul
ool
*l
ro-1
illz=282.8-284.3F: ESI SRM ms2

303.20@ | s.00 I
282.75-284.251 MS
2'tu9
.E
C:\j(calibur\...\Negative ton\21650 o70Zc->
00-1
*l
o^J
^n-l
/0
-I6p
02/16/07 09:36:53
K4 extract
NL:4.52E3
.tl/z=272.5-273.5 Fi - c
NL:
29120@15.00 [
246.50-247.&,
272.50-273.501 MS
21650
rl]/z=246.5-247.5F: - c
tr/z= 325.5-326.5 F: - c
ESI SRM ms2
344.20@15.00 [
299.s0-300.50.
325.50-326.501 MS
246.50-247.50.
272.50-273.501 MS
2't 650
21650
vnf*
,{\
100-l
o
o
o-
%
: 1.07E5
rniz= 311.5-312.5 F: - c
ESI SRM ms2
*t
*l
*l
356.00@15.00 [
311.50-312.501 MS
6!
21
ro-l
tul
rol
*l
60i
--
.-
21550
ESI SRM ms2

291.20@15.00 [
o!
ol
-l
4,31E3
rvz= 299.5-300.5 F: - c
ESI SRM ms2
344.20@15.00 l
299.50-300.50.325.50-326.501 MS
ESI SRM ms2
".-l
5Ui
OJ
I
oo-]
*l
'o-]
L,,t 4+,q
O,\1
650
C:U(calibuA...\Negative
lon\21651 O7oZ4l
0?i16107 09:47:49
TTB
NL:0
rnlz= 272.5-273.5 F: ESI SRM ms2

291.20@15.00 [
9.39
NL:3.26E3
ftVz= 299.5.300.5 F: - c
ESI SRM ms2
344.20@15.00 [
299.50-300.50,
325.50-326.sot MS
246.50-217.W,
272.s0-273.501 MS
2't65'l
21 651
m'lr-246.*247.5 Ft - c
ESI SRM ms2
291.20@15.00 [
246.50-247.50,
272.50-273.501 MS
21651
m/z= 325.5-326.5 F: - c
ESI SRM ms2
344.20@15.00 [
299.50-300.50,
325.50-326.501 MS
21 651
c
o
o
@
@
nM'
^^/
trVz= 31 1 .$312.5 F: - c
ESI SRM ms2
356.00@1s.00 [
311.s0-312.501 MS
21651
1,t qqq
.(r\
C:\jXcalibuA...\Negative lon91
52
07
aZ a
t o 13
frg
0?J16107 09:58:44
NL:8.85E3
rnlz=272.5-273.5F:
-c
nr/z= 299.5-300.5 F: - c
ESI SRM ms2
344.20@15.001
299.50.300.50,
325.50-326.501 MS
ESI SRM ms2

291.20@15.00 [
246.50.247.50.
272.50-273.501 MS
21652
21652
:2.55E:l
ttlz= 246.U247 .5 F: - c
r/z= 325.5-326.5 F: - c
ESI SRM ms2
s44.20@15.00 [
299.50-300.50,
325.50-326.50t MS
ESI SRM ms2

291.20@1s.00 [
246.fi-247.50,
272.50-273.501 MS
21652
0
^r
2't652
o
o
!
o
@.
6
@
nvz= 311.S312.5 F: - c
ESI SRM ms2
356.00@1s.oo I
311.50-312.501 MS
21652
lon\21653 OToLo lo
tJ
02116107 10:09:33
TOp
Q48 extract
NL:2.67E3
NL:0
rvz= 299.5-300.5 F: - c
ESI sRM ms2
34420@'15.00 [
nnF 272.+273.5 F: - c
ESI SRM ms2
291.20@15.00 [
246.50-247.50,
272.50-273.s01 MS
21653
299.50-300.50,
325.50-326.501 MS
21653
m/z= 325.$326.5 F:
ESI SRM ms2
344.20@15.00 [
rnlz= 246.5-247 .5 F: - c
ESI SRM ms2
2s1.20@15.00 [
246.50-247.50,
272.s0-273.501 MS
21653
-c
299.50-300.50,
325.s0-326.s01 Ms
2'1653
-'
0rg
NL: '1.29E5
rVz=311.$312.5 F: - c
ESI SRM ms2
356.00@15.00 {
311.50-312.501 MS
,IAEt
qqb
C:XcalibuA...\Negative lon\21654 OTOZOI
tg
02116107 10:20'.25
NL:0

NL: 7.30E3
nvz= 299.5-300.5 F: - c
ESI SRM ms2
344.20@15.00 [
299.50-300.50,
325.50-326.501 MS
21654
tr,lz= 272.5-273,5 Fi - c
ESI SRM ms2
291.20@15.00 [
246.50-247.50.
272.50-273.s0t MS
21654
NL:3.87E3
mlz= 246.5-247.5 Fi - c
ESI SRM ms2
291.20@15.00 [
m/2= 325.5-326.5
325.5
F: - c
ESI SRM ms2
344.20@15.00 I
299.s0-5oo.so.'
32s.s0-326.s01 Ms
246.50-247.50.
272.50-273.50i MS
21654
o
o
6
E
Al.}"
rnlz= ?42.9-28/..3 F: - c
ESI SRM rru2
303.20@15.00 I
282.75-284.25t MS
2'1654
A. rt{,.]
Z',
r.q\
00-
*l
"J
'1J
lon\21655 OToLOl
B {f p
021'16107 10:31:22
NL:3.11E3
NL: 1.57E3
.r'lz= 272.5-273.5 F. - c
299.5-300.5 F: . c
ESI SRM ms2
344.20@1s.00 [
299.50-300.50.
325.50-326.50t MS
r/z:
ESI SRM ms2
291.20@15.00 [
246.50-247.50.
272.50-273.501 MS
21655
21655
2.41e3
: 4.05E3
ftilz= 246.+247 .5 F: - c
ESI SRM ms2
291.20@1s.00 [
246.50-247.50,
272.50-273.501 MS
21655
n/z= 325.5-326.5 F: - c
ESI SRM ms2
344.20@15.00 I
299.s0-300.50.
325.50-326.501 MS
21655
Ay
-a
%
|.04E4
.r.lz=282.8-2E/.3F'. - c
r/z= 311.S312.5
ESI SRM ms2
ESI SRM ms2

3s5.00@15.00 [
303.20@15.00 [
242.75-2U.251 MS
21655
F: - c
311.50-312.s01 MS
21655
Al\l'I,
ll*,/v
(l,gr"\
C:XcalibuA...\Negative
iool
lon\21656
oaoLolol 3 JDp
0?/16107 10:42:14
NL:1.29E5
nlz-272.1273s
it
"'lI
'tl
NL: 3.25E4
F: - c
r/z= 299.5.300.5 F: - c
ESI SRM ms2

291.20@1s.00 [
246.50-247.50,
ESI SRM ms2

344.20@15.00 [
299.50-300.50.
325.s0-326.501 MS
2't655
272.5S273.501 MS
21656
8.1
100-l
"-l
q
8s-..1
*.1
'l
ro-l
*l
8.1
@
AM/
0E3
n{z= 246.5-247.5 F: - c
rvz= 325.5-326.5 F: - c
ESI SRM ms2

291.20@15.00 [
246.50-247.50,
272.50-273.501 MS
21 656
ESI SRM ms2

344.20@15.00 [
299.50-300.50,
325.50-326.501 MS
21656
@N
e
o
ol
*1
30-J
l
2s1
I
7.0185
tuz= 282.8-2U.3 F: - c
ESI SRM msz
303.20@15.00 [
282.7U2U.251 MS
21
5--lo
656
5.21E4
r/z= 311.4312.5 F:. c

ESI SRM ms2
3s6.00@1s.00 I
311.5e312.501 MS
21656
qq
( t,gz
,lr
00-l
rul
^n_.{
lon\21657
OTaLolOlS JD6
0?/16107 10:53:13
NL:4.56E3
NF272.5-273.5F:
NL:1.18E3
-c
rn/z:299.5.300.5 F: - c
ESI SRM ms2
ESI SRM ms2

344.20@1s.00 [
291.20@15.00 [
246.50-247.50,
4W.CU-JUU.JU,
272.50-273.501 MS
325.50-326.50t MS
21657
21857
:2.15E3
Irl/F246.+247.5F:-c
r/F
ESI SRM ms2

2e1 .20@15.00 [
344.20@15.00 [
299.5G.300.50.
325.5G326.501 MS
246.50-247.50.
272.50-273.501 MS
21657
2'1657
!oc
325.t326.5 F: - c
ESI SRM ms2
o
.g
&
Alv
.n/z= 282.8-2U.3 Fi - c
ESI SRM ms2
303.20@15.00 [
242.75-2U.25t MS
2'1657
Time (min)
C:XcalibuA...\Negative lon\21658
07 aZol e
021'16107 11:04:07
T-OF
NL:0
ilz= 272.5-273.5 F: . c
ESI SRM msz
291.20@1s.00 [
246.fi-247.fi,
272.50-273.501 MS
21 658
NL:0
m/z= 325.5-326.5 F: - c
ESI SRM ms2
344.20@15.00 [
299.50-300.50,
325.50-326.501 MS
21658
1001
--l
oR-J
ru-l
80-1
?5-l
to-l
ru-1
g eo_i
@
I't'v
filz= 282..*2U.3F:
1001
*l
ESI SRM ms2

303.20@15.00 [
282.7r2U.251
nol
-c
MS
21656
^-l
'-l
80-l
_-l
, t-l
tol
*l
""-l
*l
50-l
4s-]
I
oo-]
*l
ro-l
,{* qr/
(rEq
Time (min)
C:XcalibuA...\Negativelon\21659 OTCLAI
lool
ru'l
.t
Cl3 ff7
02116107 11:14:58

NL: 2.28E5
nvz= 299.5-300.5 F: - c
ESI SRM ms2
3,t4.20@15.00 [
299.50-300.50,
325.50-326.501 MS
21659
NL: 6.45E4
rrlz=272.i273.5F: - c
it
ESI SRM ms2
291.20@15.00 [
246.50-247.50,
272.50-273.501 MS
21659
NL: 1.82E4
4.33E3
246.5-247 .5 F: - c
r/z= 325.+326.5
n!z-
F: - q
ESI SRM ms2
344.20@15.00 [
299.50-300.50,
325.50-326.501 MS
21659
ESI SRM ms2
291.20@15.00 [
246.50-247.50,
272.50-273.501 MS
21 659
o
o
.E
a-14,u
NL:6.35E4
: 8.89E5
fi'lz= 2A2.a-28/..1F: - c
ESI SRM ms2
303.20@15.00 [
282.7U2U.251 MS
10(
Y'
9(
r/z=311.5-312.5F:.c
ESI SRM ms2
356.00@15,00 [
311,50-312.501 MS
21659
2t659
8!
7(
5l
4(
5(
't0
Time lminl
'l'ime (min)
C:U<'caliUurt...tNegative
lon\21660
OToLololS TrB
02116107 11.'25:5'l
NL:

NL: 6.81 E3
tt{z= 272.5-273.5 F: - c
rvz= 2995300.5 F: - c
ESI SRM ms2

291.20@15.00 [
ESI SRM ms2

344.20@15.00 I
299.50-300.50.
246.fi-247.50.
272.s0-273.501 MS
21660
325.50-326.50t MS
z toou
,oo-l
m/z= 325.5-326.5 F: . c
ESI SRM ms2
344.20@15.001
299.50-300.50,
325.50-326.501 MS
21660
ru-1
*-l
ru-l
80-l
'l
to-l
*-l
60_l
o
o
o
6
}\^\/
10(
9:
v.ocEz
filz=282.*2U.3F.-c
ESI SRM ms2
303.20@15.00 I
282.7*2U.251 MS
6.1 8E3
311 .5-3'12.5 F: - c
ESI SRM ms2
356.00@15.00 I
311 .50-3'12.501 MS
21550
r/z=
8(
7(
4Ar\l,,
c{u
qv
lon\21661 OToLol
ol? JjE
0?/16107 11:36:47
NL:3.82E3
NL:0
rilz=272.5-273.5F: -c
272.50-273.501 MS
nvz= 299.5-300.5 F: - c
ESI SRM ms2
344.20@15.00 [
299.50-300.50.
325.50-326.501 MS
2'1661
21661
rtlz=246.5-247.5 F: - c
t/z= 325.&326.5
ESI SRM ms2

291.20@15.00 [
ESI SRM ms2
ESI SRM ms2

291.20@'t 5.00 [
246.fi-247.50,
3.61E3
246.50-247.fi,
272.50-273.501 MS
21661
21661
Atl
o
.g
.e
ESI SRM ms2

3s6.00@15.00 [
3't1.50-312.501 MS
303.20@15.00 I
282.75-284251 MS
Time (min)
21661
661
li,
totr?
n/z= 31'1.5-312.5 F: . c
ntlz=282.d-284.3 F: - c
ESI SRM msz
21
F: - c
344.20@15.00 [
299.50-300.50,
325.s0.326.501 MS
Time (min)
lon\21662 OToLO/
02116107
TDtE
1:47:36
Spot LOD, 1uL Q49
1.01
NL:8.01E3
rrlz= 272.+273.5F: - c
u-63
1001
NL: 2.98E4
-m/z=
299.5-300.5 F: - c
ESI SRM ms2

2e1.20@15.00 [
246.50-247.50,
ESI SRM ms2

344.20@15.00 [
299.50-300.50.
272.s0-273.501 MS
21662
325.50-326.s01 MS
nlz= 246.5-247.5
ru-l
ESI SRM ms2

291.20@15.001
rol
246.50.247.50,
2'1662
4.02E3
rn/z= 325.5-326.5 F: - c
ESI SRM ms2
344.20@15.00 [
299.50-300.50,
325.50-326.501 MS
F: - c
272.50-273.501 MS
zt00z
--l
ztooz
*l
--l
ru-l
to-]
tt-]
to
60-l
-l
!o
5.1
0E5
1.56E5
rfl/z= 31 1.5-312.5 F: - c
ESI SRM ms2
356.00@15.00 [
311.50-312.501 MS
filz= 282.8-2U.3F: - c
ESI SRM ms2
303.20@15.00 I
282.75-2w.2sl MS
z tooz
Time (min)
c{* aV
,/ rn t:.
Time (min)
lon\21663 07o 20lo
tZ
0?/16107 11:58:29
TOg
NL: 0
NL:5.02E3
nlz= 272.5-273.5 F: - c
r/z=
ESI SRM ms2

291.20@1s.00 [
299.5-300.5 F: - c
ESI SRM ms2
344.20@15.00 [
272.50-273.501 MS
21663
325.50-326.501 MS
21663
trlz=246.5-247 ,5 F: - c
ESI SRM msz
291.20@1s.00 [
34420@15.00 [
zw,cu-Juu.il,
246.fi-247.50,
rrvz= 325.5326.5 F: - c
ESI SRM ms2
246.fi-247.50,
299.5G300.50.
325.s0-326.501 MS
21663
272.50-273.s01 MS
21 663
qv
t
o
o
:9.09E-l
10(
31 1 .$.312.5 F: . c
ESI SRM ms2
356.00@1s.00 [
311.s0-312.s01 MS
21 663
n/z=
ta
7C
oa
OL
55
c!
45
40
J!
30
Time (min)
Time (min)
C:Wcalibur\...\Negative
lon\21664 OToLtJ
olj jDB
0A17107 12:09:21
NL:7.62E3
rnlz=272.5-273.5 F: - c
ESI SRM rns2
291.20@15.00 [
246.50-247.50.
272.50-273.501 MS
216&1
1001
*-l
r,lr-248-*247.5 Fi - c
ESI SRM ms2
291.20@15.00 [
246.50-247.50.
272.50-273.501 MS
ru-l
2't664
*-1
ro-l
ru-]
70-..1
"]
60-l
Nil
1001
oaJ
;;l
*-]
nlz=282,8-2U.3F:- c
ESI SRM ms2
303.20@ rs.00 [
282.75-284.251 MS
2166/.
uo-l
--l
ro-J
'1
ro-]
*l
uo-l
ou-]
oo-]
*t
'o-]
iio vv
C:U(calibuA...\Negative lon\21665 O TOLo I a
).01
U.UJ
lj
-TDB
0?/17107 12:20:10
--l
NL:1.96E4
fflz= 272 .5-273 .5 F : - c
ESI SRM msz
291.20@15.00 [
"n-l
272.5G273.s01 MS
00-i
Spot LOD,2 uL Q49

NL: 6.38E4
ffVz= 299.5-300.5 F: -
246.50-247.50,
21665
,::
6.1 8E3
m/2= 325.$326.5 F: - c
ESI SRM ms2
344.20@15.00 [
299.50-300.50,
325.50-326.501 MS
21665
ttlz=246.5-247.5 Fi - c
ESI SRM ms2
291.20@15.00 [
246.50-247.50,
272.50-273.501 MS
21665
;.1
--l
ru-]
ESI SRM msz

344,20@1s.00 I
299.50-300.50,
325.50-326.501 MS
21 665
:f
,
"--l
ro1
ss-j
60--l
6,,P
41
10
7.c/'E4
ffi.lz=282&2U.3 F: - c
rnlz= 311.t312.5 F: - c
ESI SRM ro2
356.00@15.00 I
31'1.50-3'12.501 MS
21665
ESI SRM ms2

303,20@ r5,00 [
282.7s-2U.251 MS
21
Time (min)
665
Time (min)
C:D(cafiburl...\Negative
, t*l
lonl21666 OToLolotS Jôp
0?J17107 12:31:06
NL:4.74E3
.n'lz=272,+273.5F: . c
J./O
NL:8.98E3
rn/z= 299.$300.5 F: - c
ESI SRM msz
344.20@1s.00 {
299.50.300.50.
s25.50-326.501 MS
ESI SRM ms2
9$"]
291.20@1s.00 [
246.fi-247.50,
'.l
272.50-273.501 MS
21666
21666
n!z=246.1247.5F:- c
m/z= 325.5-326.5 F; - c
ESI SRM ms2
ESI SRM ms2

291.20@15.00 [
344.20@15.00 [
299.50-300.50,
246.50-247.50,
272.50-273.501 MS
21666
325.5G.326.501 MS
ztooo
o
P
@
ftJ
^P
ftlz=282.8-2$3F:
-c
rvz= 31 1.5-312.5 F: - c
ESI SRM ms2
3s6.00@15.00 I
311.50-312.s01 MS
ESI SRM rns2

303.20@15.00 [
282.7$284.251 MS
21666
Time (min)
2'1666
Time (min)
fnstrument Method:
EDTA_Neg_Swabs. meth
LCe fnstrument Method
Creator: Administrator
Lasr modified: z/t6/07 by Administrator
MS Run Time (min) : 10.00
Divert Valve: Dot used during run

MS
Detector Settinss:
1 fnformation
Duration (min) : 10.00
Segrment
Tune Method:
Scan Event
l_
Neg
De tails:
(291, .2 ) - >oS (246 . s-247 . s
MS/MS
2
CE L5 . 0?
IsoW
i_. 0
Neg
MS/Ms
(303 . 2) ->os (282. B-294.3)

CE 15.0? fsoW l_.0
Neg
G+e .2) ->oS (299 .5-300.

CE l-5. 0t
f soW 1. 0
MS/MS
4
EDTA_NEG
Neg
MS/MS
272.s-273 .5)
32s.s-326.s)
(3s5.0) ->oS (srr. s-312. s)

CE 15. 0t
IsoW l-. 0
Friday, February 15,
2OO7
05i :0 7 z j,4
{a 4+t-
Page 1 of
CloLc:t e 17
oz
z.o-?
Instrument Method:
EDTA_Neg_Swabs . meth
Waters 2690 LC System
Thiaafnr
narematare.
Syringe draw rate (pI/sec)

Tn'i onn i nn rrn l rrma
Drrmn
cal- f i nae
'l
\ F_ \/ '' vE
/ rr
Solvent A:80: 20 ACN:Water + 0.038

Solvent B:B
Qn l rrant
t"'1'
Solvent
D:D
Min nroccrrra
Mav nroccrrra
NH40H
.v
/PqT\
. n
\!v+,
/PqT \ . qnnn
\!vf
/.vvvv
l'hart nrrfnrrf . Droqqrrra

Ch: r1- nrrf nrri . Nn11116f
f]r:di
ont
Time
0. 00
3. 00
hrnftitm
(nin)
Flow (mI,/min)
0.30
0.30
A(r) B(r) c(E)

100. 0 0. 0
0.0
100.0 0.0 0.0
D(*)
0.
0.0
Curve
Linear
Li-near
-5
-6
Timed events:
Initial
states:
Switch L:No change
Switch 2:No change
Switch 3:No change
Switch 4:No change
ime (mi n
0.
00
Event
Switchl
Friday, February
16, 2007
Action
Parameter
No change
05:07:I4
5u q'/u
f r ar1\
Page
2 of
2
(r'/ oL<>l c-.\3
ozfrrofLaa--/
Sequenc e---07 020 1 0 1 3-Neg.sld [Open]
(neg blood, Dl H2O exl
Sample Name:
Study:
Conment:
Client:
Laboratory:
Company:
Phone:

Unknown
Sample lD
C:U(cal ibu r\Data\B rewer\07020
21634
Proc Method
lnst Method
C
Path
CalFile
:Xcal bu r\methods\E DTA-Neg-Swabs

i
Sample Vol
ISTD AMt
Dil Factor
0.u00
0.000
1.000
3\N eg
ative lon
Position
InjVol
1
I
5.0
Level
Sample Wt
1.000
Control (-EDTA blood swab ext.)
Sample Name:
Study:
Comment:
Client:
Laboratory:
Company:
Phone:

Unknown
21635
Samole lD
Path
02
:U(calibur\Data\B rewer\07020
Proc Method
lnst Method
CalFile
:Xcalibur\methods\EDTA
Samole Vol
ISTD AMt
Dil Factor
0.000
0.000
1.000
3\Negative or
I
Position
InjVol
5.0
fr aqc
b"q
page
Level
Sample Wt
0.000
Dl oL o\ ol3
a tl I ulto"1
ToP
Sequence---07 0201
3_Neg. sld [Open]
Sarnple Name: BLANK (neg blood, Dl H2O ext.)
Study:
Cornment:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
01
C:\)(calibuAData\BreweA070201
21636
Inst Method
Proc Method
Cal File
C:Xcalibur\methods\EDTA Neo Swabs

Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
3\Negative lon
Position
InjVol
5.0
Level
Sample Wt
0.000
i**************t****t****************l*****t**+**t*********************************t********i*********
Sample Name:
Study:
Comment:
Client:
Laboratory:
Company:
Phone:
mple Type File Name

Unknown
21637
Sample lD
Path
01
C:Xcalibur\Data\BreweA07020
Proc Method
Inst Method
C
Xcal
Cal File
bu r\methods\EDTA_N eg_Swabs
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
0 1 3\Negative
lon
Position
InjVol
5.0
Level
Sample
0.000
****ii*********************************************
ALrt''
/
tu
Q'la?-o lc13
4qc,
(;. i\
page2
ezfralt""l
-i-r.,p
wt
Sequence---07 0201 0 1 3_Neg.sld [Open]

Sample Name:
eltract
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Unknown
03
21638
Inst Method
Path
:U(ca|i bu AData\Brewer\O7020
Proc Method
CalFile
C:\Xcalibur\methods\EDTA Neo Swabs

Sample Vol
ISTD Amt
DilFactor
0.000
U.UOO
1.000
Sample Name:
3\Negative on
I
Position
InjVol
5.0
Level
lSample Wt
0.000
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Patn
Unknown
01
21639
Inst Method
:\Xca bur\Data\Brewer\07 020 1 013\Negative lor

I i
Proc Method
Cal File
Position
C:Xcalibur\methods\EDTA Neq Swabs

Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
q,/o
rr"
paqe 3
InjVol
5.0
ilevel
SamFte Wt
10.000
c,Tolotol3
or.l
ru I u.:.1
_J_pp
Sequence---07020
sld [Open]
0 1 3_Neg.

Study:
Comment:
Client:
Laboratory:
Company:
Phone:

Unknown
21640
Samole lD
Path
01
Proc Method
lnst Method
C
:U(calibuAData\Brewer\07020
CalFile
:Xcalibur\methods\E DTA-Neg-Swabs
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
3\N egative lon
Position
InjVol
5.0
Samole Wt
Level
0.000
*********************i*tt***********t****i***********

Study:
Comment:
Client:
Laboratory:
Company:
Phone:

Unknown
21641
Sample lD
Path
04
C: U(cali buAData\B
Proc Method
lnst Method
C
rewer\07020
CalFile
U(cal ibu r\methods\EDTA-Neg-Swabs
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
3\Negative or
I
Position
InjVol
5.0
Level
lSample
0.000
t************i**********************tt
fr qu,
(
aoz)
nan.a A
O-lol.a\ o\3
or-frc lt-oo'l
Ttf
Seq uenc e---07 020 1 0 1 3_Neg. sld [Open]

(neg blood,
Sample Name:
ext.)
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
21642
unKnown
Sample lD
Path
01
Inst Method
:U(calibuAData\Brewer\O7020
Proc Method
Cal File
101
Position

Sample Vol
ISTD Amt
Dil Factor
u.000
0.000
1.000
3\Negative I or.
InjVol
Level
5.0
Samole Wt
0.000

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
21643
Unknown
Sample lD
01
lnst Method
C
:Xcal
ib u
Path
:Xcalibur\Data\Brewer\07020
Proc Method
Cal File
r\methods\EDTA_N eg_Swabs
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
{*
3\Negative lon
Position
InjVol
5.0
++c,
(a"4)
oaqe 5
Level
Sample Wt
r0.000
01 oLolr:13
or-lrr"lr-"'1
-fl,p
Sequenc e---07 0201 01 3_Neg.sld [Open]

Study:
Comment:
Client:
Laboratory:
Company:
Phone:
File Name
Unknown
121646
Sample lD
Path
01
:Xcalibu r\Data\Brewer\07 0201 013\Negative on

I
Proc Method
lnst Method
C
Cal File
Position
STD Amt
DilFactor
0.000
0.000
1.000
Sample Wt
Level
5.0
U(ca ibu r\method s\EDTA_N eg_Swabs
Sample Vol
InjVol
0.000
************t****l

Study:
Comment:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
06
21647
Proc Method
lnst Method
C : U(ca I ibu
:\Xcali bu r\Data\Brewer\07 0201 01 3\Negative on

I
Cal File
r\methods\E DTA-N eg-Swabs
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
Position
InjVol
5.0
Level
lSamole Wt
r0,000
t***t*************************
*************
n( ,/!G
tr,t)
page 7
Cl o'yo\ olJ
or I ic f r-o. '7
TDP
Sequence---070201
3_Neg.sld [Open]

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
01
C:U(calibuAData\Brewer\07020
21648
lnst Method
C
:Xcali
bu
Proc Method
Cal File
r\method s\EDTA_Neg_Swabs
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
3\Neqative lon
Position
InjVol
5.0
Sampre
Level
wt
0.000
t*t******************s**********tt**tr********s*r***********************
(neg blood,
Sample Name:
ext.
Study:
Comment:
Client:
Laboratory:
Company:
Phone:

Unknown
21649
Sample lD
Path
01
Inst Method
C
:\Xcalibu r\Data\Brewer\07 0201 01 3\Neg ative on
Position
Xcali bur\method s\EDTA_N eg-Swabs
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
f,
'-/4 G
(t"4
page
InjVol
Level
Sample Wt
b.L)
10.000
o-lot-a
1o 1 3
"v!t elvol
Tvp
Sequence--07020
3_Neg.sld [Open]

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
07
21650
lnst Method
:U(calibu AData\Brewer\07020
Proc Method
CalFile
C:U(calibur\methods\EDTA Neo Swabs

Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Sample Name:l BLANK (neg
DI
3\Neoative
lo n
Position
lnjVol
5.0
Samole Wt
Level
0.000
ext.)
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
01
21651
lnst Method
:Xcal ibur\Data\Brewer\07 0201
Proc Method
CalFile

Vol
0.000
ISTD Amt
Dil Factor
0.000
1.000
3\Neoative on
I
Position
lnjVol
5.0
{n'/+((^" r)
oaoe 9
01
Level
lSample
0.000
a1cl/ol
o l?
crlrcfi-.'1
-5bp
Wt
Sequence---07020
3_Neg.sld [Open]
Sample Name:
Study:
Comment:
Client:
Laboratory:
Company:
Phone:

Unknown
21652
Sample lD
Path
01
C:XcalibuAData\Brewer\070201
Proc Method
lnst Method
C
Cal File
:U(cal i bu r\methods\EDTA_N eg_Swabs
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
01
3\Negative lon
Position
lnjVol
5.0
Sample Wt
Level
0.000
l********t*****************t*****t*****tt*f*********************i***************************************t*t****r**ti***

Study:
Comment:
Client:
Laboratory:
Company:
Phone:

Unknown
21653
Sample lD
Path
08
Proc Method
lnst Method
C
Cal File
:XcalibuAmethods\EDTA_Neg_Swabs
Samole Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
3\Negative lon
Position
lnjVol
5.0
{ q(L,
(t.D
oaqe 10
Level
lSamole Wt
10.000
0"1 eLol alT

oultd f r'.'"1
1vP
Seq uenc e---07 020

Sample Name:
(neg
3_Neg. sld [Open]
ext.)
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
01
C:XcalibuAData\Brewer\070201 01 3\Negative ton
21654
lnst Method
C: U(cal
Proc Method
Cal File
Fosition
ibur\methods\E DTA_Neg_Swabs
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Sample Name:
InjVol
5.0
Level
Sample Wt
0.000
K (neg blood, Dl H2O ext.)
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
mple Type File Name
Sample lD
Path
C
Unknown
21655
01
Sample Vol
ISTD Amt
Dil Factor
U.UUO
0.000
1.000
U(cali bu r\Data\Brewer\07 0201 01 3\Neg ative
{, q+.
(ao'j)
naoe
or
cloLot o t3
czlt' lto"1
-pP
Sequence---07 0201
Sample Name: Pos.
3_Neg. sld [Open]
ext.
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
09
21656
Inst Method
C
:U(calibuAData\Brewer\07 0201 013\Negative lon
Proc Method
CalFile
Xcalibu r\methods\EDTA-Neg_Swabs
Sample Vol
0.000
STD Amt
0.000
Position
InjVol
b.0
Level
Sample Wt
U.OUO
Dil Factor
1.000
Sample Name BLANK (neg blood,
ext.)
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
01
21657
Inst Method
Proc Method
CalFile

Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Position
I
3\Neqative lon
InjVol
5.U
Sample Wt
t0.000
******l*******************ff*************************#******t*************************
{o uo,
(;t)
oaoe 12
AloLcl al?
olltclr".1
5up
Sequenc e--07 0201

Sample Name:
3_Neg. std [Open]
Comment:
Study:
Client
Laboratory:
Company:
Phone:
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
****t*****tt*******trt******t*******************
Sample Name: Pos. Cont. B (Q49 ext.

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Unknown
10
21659
Inst Method
:
Path
;:xcattbur\Data\Brewer\O70201
Proc Method
U(cal i bu r\method s\E DTA_Neg_Swa6!
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Cal File
3\NEetivelon
Position
InjVol
10
5.0
Level
Samtte Wt
U.
*******************************************************t******
o-?oLol
{n 4(A
( Jt t;
r""
l3
aLlrclb-1
.TVF
Sequence---07 0201 0 1 3_Neg. sld [Open]

Comrnent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
01
21660
Inst Method
:Xcali bur\Data\Brewer\07020
Proc Method
Cal File
C:\Xcalibur\methods\EDTA Neo Swabs

Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
Sample Name: BLANK (neg
01
3\Negative on
I
Position
InjVol
5.0
Level
Sample Wt
U.OUO
elit.
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
sampre rype Frle Name
Sample lD
Path
Unknown
01
C:U(cali bu r\Data\BreweA07020
21661
lnst Method
Proc Method
CalFile

Sample Vol
ISTD
0.000
0.000
Amt
01
3\N eg
ative on
I
Position
InjVol
5.0
Level
lSamole Wt
0.000
lDil Factor
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Study:
Client:
Laboratory:
Company:
Phone:
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
t*t*************************t*f***************************t***t********t*****************************#*****************************r******
Sample Name:
Comment:
Study:
Client:
Laboratory:
Company:
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21663
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101
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0.000
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Path
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Sample Name:
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K (neg blood, Dl H2O extJ
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
sample vol
ISTD Amt
DilFactor
0.000
u.u00
1.000
**************************************t*****i**t**************i***t*******************t**t********r*****************************************
Sample Name: Spot LOD, 2 uL

Comment:
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Client:
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Company:
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C:U(calibuAData\Brewer\0702O1
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Level Sample lD
Sample Name
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Unknown
02
Unknown
03
t(2 extract
Unknown
04
Q46 extract
Unknown
05
K3 extract
Unknown
06
Q47 extract
Unknown
07
K4 extract
Unknown
08
Q48 extract
Unknown
09
10
Unknown
10
11
Unknown
11
SpotLOD, luLQ4g
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Unknown
12
Spot LOD, 2 uL Q49
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FBI Laboratory
Chemisry Unit
Toxicolory Subunit
Tox 4 I 3-0.doc
Issue Date: 0Zll5/07
Revision: 0
Page
I of9
Analysis of EDTA in Dried Bloodstains

1 Introduction
The collection of blood at crime scenes and for legal proceedings is
a common practice that may
be used to inculpate or exculpate individuals susp;ct;d of being
involved in the-crime.
occasionally, there are allegations that blood evidence collecteO f.or crime
scenes was ,,planted',.
This issue may be resolved by the determination of exogenous components in
the bloodstains (e.g.
preservatives) that should not be present in authentic crime scene evidence.
Ethylenediaminetetraacetic acid (EDTA) is an anti-coagulant and enzyme inhibitor

that is
commonly used in blood specimen collection tubes. Blood specimen collection tubes
containing
EDTA have lavender-colored tops and are the most common collection tube used to collect
reference specimens for DNA testing. Therefore, most allegations of blood evidence ,,planting,,
focus on EDTA-preserved blood samples.
EDTA-preserved blood tubes use either the disodium, dipotassium, or tripotassium salt
forms of
EDTA. The concentration of EDTA in its free acid form in a drawn blood tube is fypically
1000-2000 mg[-, depending on the volume of blood and the capaciry of the tube. At
this
concentration, the free acid and salt forms of EDTA are soluble in the blood. EDTA readily
forms
water-soluble chelates with nearly all heavy metals, so aqueous extractions of dried
blooditains
should isolate EDTA.
Scope
This procedure allows for the screening and confirmation of EDTA in suspected blood
stains.
3 Principle
This method takes advantage of the water solubilify of EDTA and EDTA-complexes.
A dried
bloodstain is first extracted with deionized water and then subjected to ultrafiltiation. Following
ultrafiltration, the filtrate is analyzed by liquid chromatography/mass spectrometry/mass

spectrometry (LCA4SA4S) in both the positive and negative electrospray ionization (ESI)
modes.
4 Specimens
This procedure can be used for assaying bloodstains from a cotton swab or other
cotton-based
matrices.
This is an uncontrolled copy of a controlled document.
n qlb
FBI Laboratory
Chemistry Unit
foxicology Subunit
,,,,.;lJ,oji;lro,;;
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Eq
uipmen t/lVlaterials/Reagents
Guidance for the preparation of reagents may

be found inthe preparation of chemical
Reagents
standard operating procedure
flox iO:).
a'
Liquid chromatograph/mass spectrometer equipped

with a Hamilton pRp-l polymeric
x 5pm) or equivalint
column (2.I mm x 150 mm

b.
Laboratory scissors
Millipore Amicon ultra-4 10,000 Molecular weight

cutoff centrifugal Filter Device
d.
Wheaton (or similar) pipette
e.
Centrifuge
f.
EDTA-preserved whole blood
200 pL
EDTA-free whole blood

Deionized water
Acetonitrile (HPLC grade)

Ammonium Hydroxide (HPLC grade)
Deionized water (9s%) / Acetonitrire (s%) / Ammonium
Hydroxid e (0.06%)_ Mobile
Phase for Positive Electrospray Ionization
Acetonirrile (80%) / Deionized water (20%) / Ammonium

Hydroxid e (0.03%)_ Mobire
Phase for Negative Electrospray Ionization
Common laboratory supplies such as glassware, pasteur
pipettes, etc.
6 Standards and Controls

EDTA LCA4S/MS(ESI) performance Mix_ 100 pglml-:
Accurately weigh r2.7 mgof the disodium saltofE-DTA
(reagent grade, Ardrich) and
dilute with deionized water to a final volume
of 100 rnr. btoie at room temperature in a
clear glass container. Stable for at least 6 months.
{u/\ uut
(,) /,;\
FBI Labontory
Chemisrry Unit
Toxicology Subunit
Tox 413-0.doc
Issue Date:.02l15/07
page 3 of 9
b.
dr2-EDTA Working Internal Standard Solution _

500 pglml:
Accurately weigh 5 mg of the free acid of drz-EDTA
i.;d";;grade, cambridge Isotope
Laboratories) and dilute with deionized water
to a finar vJlu*Jor l0 mL. store frozen
in
a brown glass container. Stable for at least
6 months.
Negative Bloodstain Control:
Add 50 pL of EDTA-free whore brood to a cotton-tip
appricator. Dry for at least 30
minutes at room temperature before use. Store
at room temperature in a glass test tube
or
paper envelope. Stable for at least 2 yeus.
d.
Positive Bloodstain Control :

Add 50 pL of EDTA-preserved whole blood to a cotton-tip
applicator. Dry for at least 30
minutes at room temperature before use. Store at room
t..p.iutur. in a glass test tube or
paper envelope. Stable for at least 2 years.
7 Calibration
This procedure has not been validated for quantitative
analysis.
8 Sampling
Not applicable.
9 Procedure
a.
carefully cut the tip from a cotton swab (negative control, positive
control, or questioned
swab) using clean laboratory scissors.
b.
Place the cotton swab tip into a separately labeled

molecular weight cutoff filter device.
Add 200 pL of the drz-EDTAWorking Internal standard

Solution directly to each cotton
swab tip in the molecular weight cutoff filter device.
Allow to sit at room temperature for
45 minutes.
d.
centrifuge the molecular weight cutoff firter device

for l0 minutes atz500RpM.
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'*''r'i:%:li:::
Issue Date: 02/15/07
ff;:l?3
e'
Transfer the filtrate to an autosampler vial and inject 5 pL

into the LClIr4S/lr4S system that
is in negative ion mode and monitor for both the free acid
of EDTA and the
EDTA-iron
complex.r SuTll:l that screen positive are confirm.o Ly in;..tion
of 5 pL of the filtrate
into the LClIr'IS/l\4S system in the positive ion mode, in wtrich
the free acid of EDTA can
De conllrTned.
l0 Instrumental
Conditions
10.1 Liquid Chromatograph parameters

10.1.1 Positive Electrospray Ionization Mode
Mobile Phase Composition: Deionized Water (95%) / Acetonitrile (5%)
/ Ammonium Hydroxide
(0.46%)
Column Parameters: Hamilton PRP-I (2.I mm
x 150
mm x 5pm) at ambient temperature
Isocratic Flow Rate: 0.3 ml/minute
10.1.2 Negative Electrospray lonization Mode

Mobile Phase composition: Acetonitrile (80%) / Deionized water (20%) / Ammonium
Hydroxide
(0.03%)
Column Parameters: Hamilton PRP-l (2.1 mm
150 mm x 5pm) at ambient temperature
Isocratic Flow Rate: 0.3 mllminute
10.2 Mass Spectrometer Parameters

10,2.1 Positive Electrospray Ionization Mode
Spray Voltage: 4.5 kV
Capillary Temperatur e: 230" C

Capillary Voltage: +30V
Collision Induced Dissociation: 100%
'
See note on carryover in the
Limitations section of this procedure (Section l4).
This is an uncontroiled copy of a controiled document.
L-\a ,\Y'r \r
FBI Laboratory
Chemistry Unit
Toxicology Subunit
Tox 413-0.doc
Issue
Date:
02/15107
Revision: 0
Page 5
MSA4' Mode:
orog:*::f
Collision Energy =
m/z 293.0(EDTA Free
Acid))
(m/z 125.0-
15.0%62
of9
ls.0);
Acquisition Time: l0 minutes

10.2.2 Negative Electrospray Ionization Mode
Spray Voltage: 4.5
kV
Capillary Temperatur e: 230" C

Capillary Voltage: -10V
Collision Induced Dissociation: 0% (Offl
SRM
Mode: All Collision Energies

Segment
I (EDTA
Set
Free
to l5%
Acid): m/z 291.2 ) (m/z 246.5-247.5; m/z 272.5-273.5)
Segment 2 (dr2-EDTA Free Acid): m/z 303.2
(m/zzg2,g-2s4.3)
Segment 3 (EDTA Iron Complex): m/z 344.2
(m/2299.5-300.5;m/z 325.5-236.5)
Segment 4 (d'2-EDTA Iron complex): m/z 356.0
(m/z3lr.5-312.5)
Acquisition Time: 10 minutes
11 Decision Criteria
11.1 Performance Mix Suitability
Proper calibration and sensitivity of the LCII\4S/MS (ESI) are demonstrated
each day samples are
analyzed. The EDTA LCll\4SA4S (ESI) Performance Mix effectively
evaluates rvrr* suitability.
Proper mass assignments' elution times, and signal-to-noise responses
can be assessed by
analyzing 5 pL of the Performance Mix. In all instances, the elution
time should be +zyoof the
retention time (relative or absolute) obtained from the previous run's
injection of the performance
Mix' A stacked Gaussian-shaped peak must be pr.r.ni for the EDTA Free Acid anallte
with a
signal-to-noise ratio exceeding 50:l for all extracted ions.
'
m/z 160 and247 are monitored for EDTA confirmation.
/'
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FBI Laboratory
Chemistry Unit
t*''r"i:%::l:::
Issue
Darc: 02/lS/07
Revision:0
Page 6
of9
11.2 Analyte Suitabitify

The following criteria are used as guideline_s in determining the acceptabilify
of the data produced
in this assay. In general, compound identification should 6e based on
a comparison of the
chromatography and mass spectrometry for the analyte peak of interest
with data from a
contemporaneously analyzed reference standard or extracted Positive Control.
In most cases, all
of the following should be met in order to identi8, EDTA within a bloodstain:
ll.2.l
Chromatography
The peak of interest should show good chromatographic fidelity, with reasonable peak
shape,
width, and resolution. Additionally, the following two criteria should be met:
ll,2.l,l
Retention Time
The retention time of the peak should be within +ZYo of the retention time (relative
or absolute)
obtained from injection of the EDTA LCA4S (ESI) Performance Mix, extracted positive
control,
or the drz-EDTA internal standard.
11.2.1.2 Signal-to-Noise
justify the existence of a peak, its signal-to-noise ratio must exceed 3. Further,
the baseline
signal for the peak from the sample of interest must be at least l0 fold greater than that
for any
observed peak at a similar retention time in a Negative Control or blanf sample injected just
prior
to that sample.
To
11.2.2 Mass Spectrometry

The mass spectral results (whether run in SRM mode or full scan products mode) for
the analyte
of interest should match that ofthe appropriate reference standard or an extracted positive
Control
within a reasonable degree of scientific certainty. See the Guidelines
for Comparison of Mass
spectra standard operating procedure (Tox 104) for further guidance.
l2
Calculations
Not applicable.
f- +v t-,
,r
a\
FBI Laboratory
Chemistry Unit
Toxicology Subunit
Tox 413-0.doc
Issue
Date: 02/15/07
Revision: 0
Page 7
of9
13 Uncertainty of Measurement
Not applicable.
l4
Limitations
a'
the
Limit of Detection (LoD): The LoD for EDTA was determined to be

13 pglml in both
positive and negative electrospray ionization modes. These
detection limits were
determined by triplicate analysis of serial dilutions of an EDTA
solution. The lowest
concentration that reproducibly met the decision criteria listed in Section
l l above was
determined to be the LOD.
separate LoD study was conducted to determine the minimum volume

of
EDTA-preserved blood that was detectable using this analytical method.
Three milliliters
of whole blood were placed into a 4-mL lavendei-topped blood collection
tube containing
7'5 mg of EDTA and thoroughly mixed. The EDTA-prbserved blood was placed
on a clean,
non-porous surface in triplicate at the following volumes: I pL, 5 pL, and
l0 pL.
Following a I -hour drying period, the blood stains were swabbed using deion
lzed water
and cotton-tipped applicators. Each swab was extracted and analyzedio
determine the
minimum sized EDTA-preserved blood stain required in order to detect EDTA
on the swab
using the decision criteria requirements of Section I l. The I pL drop was
readily
detectable using this technique.
b.
Selectivity: Selectivity was determined by extraction and analysis of l0 matrix

blanks
(swabs dipped into different blood samples with a variety of non-EDTA
preservatives
added to them). None of the l0 matrix blanks exhibited peaks of EDTA
ihat met the
decision criteria requirements of Section I
Additionally, d12-EDTA was evaluated for
interferences in the analysis and none was observed.
l.
Matrix Effects: Five extracted matrix blanks were spiked with an equal amount
of an
EDTA standard at both low and high concentrations. Following analysis of these
samples,
the results were compared with equal concentrations of neat pOfe to
determine the
amount of ion suppression caused by the blood matrix. While ion suppression
was not
noted in the positive electrospray ionization mode, suppression of 3%
ind34olo were noted
in the negative electrospray ionization mode at EDTA ioncentrations
of 50 pglmLand 500
p,g/mL, respectively.
d.
Carryover: It has been reported in the literature that trace amounts of EDTA
may be
absorbed in the chromatographic system and released in a subsequent
analysis of a sample.
This carryover was assessed during validation, but was determined to
be minor in nafure
appearing mainly after the injection of a high concentration of EDTA.
To demonstrate the
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Issue Date:
02/lS/0i
il:lT,3
lack of carryover within an analytical run, a minimum of two matrix-matched
negative
samples (i.e. whole blood extracts) must be analyzed between case samples.
15 Safety
Take standard precautions for the handling of chemicals and biological materials.
Refer to the FBI
Laboratory Safety Manual for guidance.
16 References
Miller, M.L., Mccord, 8.R., Martz, R., and Budowle, B. "The Analysis of EDTA in Dried
Bloodstains by Electrospray LC-MS-MS and Ion Chromatography", Journal of Analytical
Toxicologt, Vol. 2 l, 1997, 521 -528.
Sheppard, R.L. and Henion, J. "Determining EDTA in Blood", Analytical Chemistry,Vol. 69,
1997,477A-480A.
Preparation of Chemical Reagents (Tox 103); FBI Laboratory Chemistry Unit

Subunit SOP Manual.
- Toxicology
Guidelinesfor Comparison of Mass Spectra (Tox 104); FBI Laboratory Chemistry Unit
Toxicology Subunit SOP Manual.
FBI Laboratory Chemistry Unit - Instrument Operation and Support Subunit SOp Manual.
FBI Laboratory Safety Manual.

|
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4 4> )
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FBI Laboratory
Chemistry Unir
Toxicology Subunit
Tox
Issue
Datc:
l-0.doc
02115107
Revision: 0
Page 9
Rev, #
Issue Date
02/15t07
ol'9
New document.
Approval
Chemistry Unit Chief:
O{/a^-FgMarc A. LeBeau
OA Approval
n/r.ln
oate:4lSllOOT
Quality Manager:
Issuance
Tox Subunit Manager:

Madeline A. Montgomery
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lnst 202-0.doc
Page I ofS
Performance Monitoring protocol (eA/eC)

for the Finnigan LCe LCIMS (ESI)
Scope
This document addresses the performance monitoring (QA/QC)

of the Finnigan LCe LCA{S
system consisting of a Finnigan LCQ MS and a waters LC. it ls
an analytical instrument used to
analyze a wide variety of evidence and must be maintained in such
u *uy as to verify its
reproducibility from analysis to analysis and its reliability in court.
2 Principle
The LCQ system is comprised of a Waters Liquid Chromatograph (LC) and
a Finnigan ion trap
LCQ Mass Spectrometer (MS). The instrument is configurei with an ApI
source th-at is capable
of both electrospray (ESI) and atmospheric pressure chemical (APCD ionization.
The
instrument is primarily used in ESI mode. However, this protocol can also
be used for ApCI
provided the method of ionization is clearly labeled in the resulting
data and documentation.
Definitions and guidelines for following this protocol are outlined in the ,,General
Insrrument
Maintenance Policy."
E q u i p m en
t/UIateria ls/Rea gen ts
a.
Instrumentation - Finnigan LCQ MS, API Source, Waters Alliance 2690/2695

LC,
and Data System with XCalibur software (or equivalent)
b.
API Gas - Nitrogen, 9999% (high purity or equivalent)

Ion Trap Gas - Helium,99.99%o (high purity or equivalent,l
d.
Methanol, HPLC grade
e.
Deionized Watero 18 MO
Milli-e
or equivalent
Acetonitrile, HpLC grade

g
Acetic Acid, reagent grade
{x
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l"D
FBI Laboratory
rnsrrument opera,,..
* s:|;TigoYil:
Inst 202-0.d0c
Issue Date:06/21106
page 2 of 8
h.
Ultramark 1621 (Finnigan or equivalent)
t.
Caffeine (Sigma or equivalent)
j.
MRFA (L-methionyl-arginyl-phenylalanyl-alanine acetate) (Finnigan

or equivalent)
k.
Ammonium Hydroxide (l.lH4OH), reagent grade
t.
Codeine (Sigma or equivalent)
Brucine (Sigma or equivalent)

n.
Reserpine (Sigma or equivalent)
Volumetric glassware
h
|'.
Infusion syringe - l0 to 500 pL LC syringe (Hamilton or equivalent)

4.1 Testmix
The Testmix is used to assess daily operating performance, mass assignment,
and continued
integrity of the system. To prepare, weigh 5.0 mg caffeine, 1.0 mg cod.in",
1.0 mg brucine, and
1.0 mg reserpine into a 100-mL volumetric flask. Bring to the
mark with methanol and mix well.
Store the solution in the refrigerator. It has a shelf-lifJof three years.
This preparation may be
appropriately scaled up.
4.2 Calibration Solution

The calibration solution is used for coarse tuning and calibrating the
mass spectrometer over the
entire mass range. This procedure only needs to be performed when the
instiument has been
moved, down for a long period of time, undergone i major repair,
or wananted based on system
performance.
The calibration solution is a solution of caffeine, MRFA, and ultramark
l62l in
acetonitrile:methanol:water containing l% acetic acid. To prepare this
solution, follow the
procedure in the LCQ'Getting Started'manual. Store the solution
in the refrigerator. It has a
shelf-life of three years. This preparation may be appropriately scaled
up.
{"
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FBI Laboratory
Chemisfy Unit
lnstrument Operation
& Support Subunit

Inst 202-0.doc
Issue Dale: 06/21/06
Revision: 0
Page 3 of8
5 Calibration
The calibration procedure should be performed as needed, when the instrument has been moved,
down for a long period of time, undergone a major repair, or warranted based on system
perforrnance.
a.
Load a 250 1tL syringe with the calibration solution.
b.
Using capillary tubing, connect the infusion syringe to the ESI probe assembly, and
place in the syringe pump.
c.
Set the syringe pump to the correct syringe fype and set the pump rate tolQ
pllminute.
d.
Load the tune file "ESI_TL|NE" (or equivalent).
e.
Check that instrument is in POSITIVE ION mode and collecting CENTROID data.
f.
Set the detector using the parameters listed in the 'Instrumental Conditions'section
of
this protocol.
g.
Turn on the syringe pump and verif, that the solution is flowing out the ESI needle.
h.
Engage the ESI probe and turn on the MS.
i.
j.
In Tune Plus, open the Calibrate dialog box, choose the'Automatic'tab and check the
individual tests or'Select All' and then 'Start.'
When the calibration is complete, it
successful.
o
r
k.
will display whether or not the calibration was
Ifthe
procedure fails, repeat the calibration.

When the procedure passes, print the report and evaluate the calibration
solution spectrum using the'Decision Criteria' section of this protocol. If the
results are acceptable, print the spectrum of the calibration solution.
If all requirements
are within specification, prepare the documentation as outlined in
the "General Instrument Maintenance
Policy." If any requirements fail, the IOSS
a^L 44 G
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FBI Laboratory
rnstrument operat,."
. fliTJHoYlil
Inst 202-0.doc
Issue Date: 06/2l/06
ff;:1?3
Manager
will
determine the corrective action to be taken.
6 Sampling
Not applicable.
7 Procedures
7.1 Daily Checks
The following steps are to be performed daily. Enter the appropriate information in the
log for tracking purposes.
eA/eC
a.
Record the remaining disk space on the hard drive. Use Windows Explorer program
(WindowsNT) to verifu that the hard disk has at least 100 MB of free disk space-. Do
not use if less than 100 MB remain.
b.
Record the line pressure of the building nitrogen supply (ApI gas). The regulator
should read between 60 and 100 p.s.i. If it cannot maintain thii pressure, contact
IOSS. If the nitrogen is supplied by a gas cylinder, record the tank pressure. Change
the tank if less than 100 p.s.i. remaining.
Record the line pressure of the building helium suppry (ion trap gas). The regulator
should read between 30 and 60 p.s.i. If it cannot maintain this pressure, conracr
Ioss. If the helium is supplied by a gas cylinder, record the tank pressure. change
d.
Check the Ion Gauge to ensure that no significant leaks are present in the system. Do
not use if the pressure is higher than I x l0-a torr.
e.
Prepare the instrument for analysis of Testmix. Verifu that the instrument has the
correct source probe installed (ESI), the correct tune file loaded (esi_tune or
equivalent), positive ion mode selected, and centroid data being collected. If a
column is installed, remove it from that system and replace it wittr the infusion
capillary tube.
Perform an analysis of the Testmix prior to the analysis of evidence using parameters
listed in the 'Instrumental Conditions' section of this protocol. Start the ftplC pump.
Engage the ESI probe and turn on the MS. Start an acquisition using a filenam!
such
t"
4qa
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FBI Laboratory
rnstrument operat'.,'
rililiH#lil
Inst 202-0.doc
Issue Date: 06/2l/06
lilii[!
as'testmix'(or equivalent). Make three 5 pL injections of the Testmix solution
approximately l0 seconds apart by using the manual loop injector, and
then stop the
data collection. Evaluate the results using the 'Decision Criteria'
section of this
protocol. If the results are acceptabte, print the TIC and spectra for all
components in
the Testmix.
g'
If all requirements are within specification, prepare the documentation as outlined in

the "General Instrument Maintenance Policy." If any requirements fail, contact
IOSS.
7.2 As Needed Checks

Re-cut or replace the sample capillary as needed.
b.
Clean or replace the heated capillary as needed.
8 Instrumental Conditions
Refer to the "General Instrument Maintenance Policy" for procedures on minor deviations.
8.1 Testmix
Liquid Chromatograph
Mobile Phase:
Flow Rate:
Column:
Inj Volume:
Number of Inj:
95:5 methanol:water + 0.03% ammonium hydroxide

0.2 mllmin
None
5pL
a
Mass Spectrometer
Ionization:
Tune File:
Scan Mode:
Full Scan
Scan Range:
100-650 m/z
ESI
esi_tune
{a uVt
( a st-)
I+
FBI Laborarory
Chemistry Unit
Instrument Operation
& Support Subunit

Inst 202-0.doc
Revision: 0
page 6 of g
8.2 Calibration
Mass SDectrometer
Ionization:
ESI
Tune File:
esi_tune
Scan Mode:
Scan Range:
Full Scan
100-2000 m/z
Decision Criteria
9.1 Testmix
Verifu the results of the Testmix. The following ions should be observed in the three Testmix
injections:
o Caffeine 195 m/z

o Codeine 300 mlz
r Brucine 395 mlz
. Reserpine 609 mlz
9.2 Calibration
Verify the results of the calibration. The calibration will indicate if the procedure was
successful. The individual ions for the calibration solution are:
r
o
r
Caffeine
195 mlz
MRFA
524 mlz
Ultramark 1022 mlz
ll22
m/z
1222 mlz
1322 mlz
1422 m/z
1522 mlz
1622 mlz
1722 m/z
1822 mlz
1922 mlz
greater than 5Yo

greater than 50%
greater than 5Yo
greater than 20o/o
greater than 50Yo
greater than 50Yo
greater than 80%o
greater than 50%o
greater than 50To
greater than 20%o
greater than 10%o
present
n(a (vu,
s"t)
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FBI Laboratory
rnsrrument
oprat',"
* f liTJHrYlil
Inst 202-0.doc
Issue Date: 06/21106
ff;:'il,3
10 Calculations
Not applicable.
ll
Uncertainty of Measurement
Not applicable.
12 Limitations
Only properly trained personnel shall perform duties involved in the operation, maintenance, or
troubleshooting of this instrument.
13 Safefy
Take standard precautions for the handling of all chemicals, reagents, and standards. Refer to
the FBI Laboratory Saf"ty Manual for the proper handling and disposal of all chemicals.
Personal protective equipment should be used when handling any chemical and when performing
any type of analysis. Many instrument components are held at temperatures of 250oC and
higher. Precautions should be taken to prevent the contact of skin with heated surfaces and
areas.
14 References
Manufacturer's Instrument Manuals for the specific models and accessories used.
"General Instrument Maintenance Policy" (Inst 001) Instrument Operation and Support Subunit
SOP Manual.
"Liquid Chromatograph General Maintenance Protocol" (Inst 003) Instrument Operation and
Support Subunit SOP Manual.
"Mass Spectrometer General Maintenance Protocol" (Inst 004) Instrument Operation and
FBI Laboratory Safety ManuaL
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FBI Labontory
Chemistry Unit
Toxicolory Subunit
Tox l034.doc
Revision: 2
Page I of 15
Preparation of Chemical Reagents
Scope
This procedure provides instructions for the preparation and storage of all reagents used
in the
various standard operating procedures of the Chemistry Unit's Toxicology Su-bunit. This
document does not provide information for materials used directly as obiained from the
manufacturer. Neither does it provide instructions for the preparation of calibrators, controls,
or
analytical standards. Prepared reagents are listed, in alphabetical order, in section 6, ,,procedure,,
and materials needed for preparation of these reagents are listed in section 2,o,Equipment/
Materials/Reagents." Refer to the Chemistry (Jnit Procedure
for Verification of'Re'agents, Kits,
Solvents and Standards (CUQA 9) for guidance in labeling and testing the reliabilirylf reagents.
2 Equipment/lVlaterials/Reagents
a.
Electronic balance
b.
pH paper in various ranges
c.
Ultrasonicator
d.
vacuum filtration apparatus
(l
liter size) with 0.5 pm prFE filter membranes
Miscellaneous routine laboratory glassware and supplies
Acetic acid, glacial(17 M) (ACS grade)

o
Acetonitrile (HPLC grade)
h.
Ammonium acetate (reagent grade)

Ammonium hydroxide, concentrated (15 M) (ACS grade)
J.
Calcium chloride (reagent grade)
k.
Chloramine T (reagent grade)
l.
Chloroform (GC2 grade and HpLC grade)
m,
o-Cresol (reagent grade)
{-u v+t/a
FBI LaboBtory
,"*:li"H'g#li:
Tox I 03-2.doc
rssueDate:
l:i1lf::t
Page2ofl5
n.
Cupric sulfate pentahydrate (reagent grade, CuSOa.5H2O)
o.
Curcumin (reagent grade)
p.
Diethyl ether (high purity grade)
q.
Dimethylsulfoxide (ACS grade)
r.
Diphenylamine (reagent grade)
s.
Ethyl acetate (HPLC grade)
t.
Ethyl alcohol (200 proof and pharmaceutical grade)
u.
Ferric chloride hexahydrate (reagent grade, FeCls.6HzO)
v.
Ferric nitrate nonahydrate (reagent grade, Fe(NO3)3,9H2O)
w.
Gold(III) chloride hydrochloride trihydrate (reagent grade, HAucl+.3Hzo)
x.
Heptafluorobufyric acid (aka HFBA) (reagent grade)
y.
Hexamethonium hydroxide solution, 0.1 M (obtained from Fluka Chemical Company)
z.
Hexane
aa.
Hydrochloric acid, concentrated (12 M) (ACS grade)
bb.
Indigo Carmine (reagent grade)
cc.
Iodine (reagent grade)
dd.
Isopropanol (2-propanol) (HPLC grade)
ee.
Magnesium nitrate (high purity grade I)
ff.
Mercuric chloride (reagent grade, HgCl2)
eg.
hh.
Methanol (GC2 grade and HPLC grade)
ii.
Nitric acid, concentrated (16 M) (ACS grade and optima grade)
(UV grade)
Methylene Chloride (dichloromethane) (HPLC grade)
(-s)
t/t)t
YY 2,
:?:tlHr"#
'*'1.1:?r::,::::
Issue
Date:
1012712006
Revision: 2
Page 3 of 15
jj.
Palladium matrix modifier solution (0.1% obtained from High-Purity Standards,Inc.)
kk.
PIC reagent (methanesulfonic acid) (reagent grade)
ll'
PICB-8 reagent (octanesulfonic acid) (low UV grade obtained from Waters Corp.)
mm. Potassium
cyanide (reagent grade)
nn,
Potassium ferricyanide (reagent grade)
oo.
Potassium hydroxide (reagent grade)
pp.
Potassium iodide (reagent grade)
qq.
Potassium phosphate, monobasic (ACS grade, KH2pOa)
rr.
Pyromellitic acid (reagent grade)
ss.
Saponin (reagent grade)
tt.
Silver nitrate (reagent grade)
uu.
Sodium acetate trihydrate (reagent grade)
vv.
Sodium bicarbonate (reagent grade)
ww.
Sodium borate (sodium tetraborate decahydrate) (ACS grade, NazB+oz.l0H2o)
xx.
Sodium chloride (reagent grade)
W.
zz.
Sodium dithionite (reagent grade)

Sodium hydroxide (ACS grade)
aaa.
Sodium phosphate, dibasic heptahydrate(ACS grade, Na2HpO4.7H2O)
bbb.
Sodium phosphate, monobasic monohydrate (ACS grade, NaHzpO+.HzO)
ccc.
Sulfuric acid, concentrated (18 M) (ACS grade)
ddd.
Tetramethylammonium hydroxide (ACS grade)
(/
((-
FBI Laboratory
Chemistry Unit
Toxicology Subunit
Tox 103-2.doc
Issue
Date:
10127
12006
Revision: 2
Page4ofl5
Toluene (HPLC grade)
fff.
Triethanolamine (reagent grade)
ggg.
Trifluoroacetic acid (98+% purity)
hhh.
Water, Deionized (18+MO grade)

Not applicable.
4 Calibration
Not applicable.
5 Sampling
Not applicable.
6 Procedure
Unless specifically noted otherwise, all reagents can be prepared in larger or smaller total volumes,
as needed, by appropriate scaling of component volumes and masses. Listed grades or qualities
of
chemicals are the minimum acceptable levels. Unless specifically noted otherwise, a higher
quality of the same chemical may be substituted.
a.
50 mM Acetic Acid:
To a 100-mL graduated cylinder, add 80 mL deionized water and 0.25 mL glacial acetic
acid. Mix well and bring to 85 mL with deionized water. Store in glass at room
temperature. Stable 3 months.
b.
0.1 M Acetic Acid:

To a 100-mL graduated cylinder, add 80 mL deionized water and 0.5 mL glacial acetic acid.
Mix well and bring to 85 mL with deionized water. Store in glass at room temperature.
Stable 3 months.
. qVL
ss)
FBI Laboratory
Chemistry Unit
Toxicology Subunit
lssue
Tox I 03-2.doc
Date: 10/27/2006
Revision: 2
Page5ofl5
Dilute
(-
1.5 M) Acetic Acid:

Mix 2 mL glacial acetic acid with 20 mL deionized water and shake to combine. Store in
glass at room temperature. Stable 3 months.

d.
I Acetonitrile:Water:
Combine 100-mL HPLC grade acetonitrile with 100 mL deionized water and mix well.
Store in glass at room temperature. Stable 6 months.
0.1 M Ammonium Acetate:
Add 3.85 g ammonium acetate to a 500-mL volumetric flask containing 300 mL deionized
water. Mix well to dissolve, and bring to volume with deionized water. Store in
refrigerated in glass. Stable 2 months.
0.24 M Ammonium Hydroxide:
Add 1.6 mL concentrated ammonium hydroxide to 50 mL deionized water in a 100-mL
graduated cylinder. Fill to the 100-mL mark with deionized water and mix well. Store
in
glass at room temperature. Stable
I month.
o
b.
2 M Ammonium Hydroxide:
Add l0 mL concentrated ammonium hydroxide to 50 mL deionized water in a 100-mL
graduated cylinder. Fillto the 75-mL mark with deionized water and mix well. Store in
glass at room temperafure. Stable I month.
h.
5% (wlv) Calcium Chloride Solution:

Dissolve I g calcium chloride in 20 mL deionized water. Store in glass at room
temperature. Stable I year.
CE (Capillary Electrophoresis) Run Buffer - Anions:
To a 1000-mL volumetric flask, add 500 mL deionized water, 612 mgpyromellitic acid,
280 mg sodium hydroxide, 238 mg triethanolamine, and 7.5 mL 0.1M hexamethonium
hydroxide solution. Mix wellto dissolve, and bring to volume with deionized water. Store
refrigerated in plastic. Stable I week.
05% (wlv) Chloramine T:

To a 100-mL volumetric flask, add 80 mL deionized water and 0.5 g chloramine T. Mix
well to dissolve and bring to volume with deionized water. Store refrigerated in glass.
Stable 6 months.
k.
4:
I Chloroform:Methanol:
Combine 40 mL GC2 grade chloroform with l0 mL GC2 methanol. Mix

brown glass at room temperature. Stable I month.

'\ '14 L,
Zr
{s t+\
well.
Store in
FBI Laboratory
Chemistry Unit
Toxicology Subunit
Tox 103-2.doc
Issue
Date:
10127/2006
Revision: 2
Page 6 of l5
l% (by volume) o-Cresol:

Place I mL o-cresol in a 100-mL volumetric flask and fill to the mark with deionized water.
Mix well and allow to stand for at least 24 hours before use. Store refrigerated in brown
glass. Stable 6 months.
m.
5% (w:v) Cupric Sulfate Solution:

Dissolve 1.56 g cupric sulfate pentahydrate in 20 mL deionized water. Store in slass at
room temperature. Stable I year.
n.
Curcumin Solution (saturated in ethanol):

Add curcumin to l0 mL 200 proof ethanol in a test tube with mixing until no more will
dissolve. Centrifuge at low speed for 5 min and transfer the supernatant. Store in glass at
room temperature. Stable 1 year.
Cyanmethemoglobin Reagent (Drabkin's Solution):
To a 1000-mL volumetric flask containing 500 mL deionized water, add 200 mg potassium
fenicyanide, 50 mg potassium cyanide, and I g sodium bicarbonate. Mix well to dissolve
and bring to volume with deionized water. Store refrigerated in brown glass. Stable 4
months.
p.
q.
Diphenylamine Reagent (05% w:v in sulfuric acid):

Dissolve 0.5 g diphenylamine in 100 mL concentrated sulfuric acid. Store in glass with
PTFE-lined cap at room temperature. Stable I year.
80% (by volume) Ethanol:

Measure 80 mL pharmaceutical grade ethanol into a 100-mL volumetric flask. Bring to
volume with deionized water and mix well, Store in glass at room temperature. Stable for
6 months.
l:l
Ether:Toluene:
Combine 50 mL HPLC grade toluene with 50 mL diethyl ether. Mix
at room temperature. Stable I month.
well.
Store in slass
5% (wlv) Ferric Chloride Solution:

Dissolve 1.67 g fenic chloride hexahydrate in 20 mL deionized water. Store in slass at
05% (w/v) Gold Chloride Solution:

Dissolve 130 mg gold(IID chloride hydrochloride trihydrate in 20 mL deionized water.
Store in brown glass at room temperature. Stable I year.
a^t 4( b
/ j,/c,\
:?:*1'f,11'#
'*111?,::*::
Issue
Date: l0n7/2006
Revision: 2
PageTofl5
u.
0.1% (w/v) Heptafluoroburyric Acid:

Add 0.5 g HFBA to 400 mL deionized water in a 500-mL volumetric
flask and mix well.
Bring to volume with deionized water. Store in glass at room temperature.
Stable 3
months.
2mM Hydrochloric Acid:

In a 100-mL volumetric flask, combine g0 mL deionized water with l6 pl
concentrated
hydrochloric acid and mix well. Bring to volume with deionized water.
Store in glass at
room temperature. Stable 6 months.
w.
0.1 M Hydrochloric Acid:
To a 100-mL graduated cylinder, add 80 mL deionized water and 0.8 mL concentrated

hydrochloric acid. Bring to 96 mL with deionized water and mix well. Store
in slass at
room temperature. stable 6 months.
X,
0.96 M Hydrochloric Acid:
To a 100-mL volumetric flask, add 80 mL deionized water. Add S mL concentrated

hydrochloric acid and mix well. Bring to volume with deionizedwater. Store glass
in
at
v.
I M Hydrochloric Acid:
To a 100-mL graduated cylinder, add 80 mL deionized water. Add 8 mL concentrated
hydrochloric acid and mix well. Bring to 96 mL with deionized water. Store glass
in
at
M Hydrochloric Acid (- 50% v:v):

To a 25-mL graduated cylinder containing l0 mL deionized water, add l2 mL
concentrated hydrochloric acid and mix well. Bring to 24 mLwith deionized
water. Store
in glass at room temperature. Stable 6 months.
6
aa.
0.01% (w/v) Indigo Carmine Reagent:

Dissolve l0 mg indigo carmine in 100 mL deionized water. Store in glass at room
temperature. Stable I year.
bb.
Iodine Test Solution:

Dissolve 0.4 g iodine and 0.6 g potassium iodide in 20 mL deionized water.
Store in qlass
at room temperature. Stable 6 months.
LC (Liquid chromatography) Mobile phase

methanol :water:ammonia)
- Alkaline#l / cocaine (95:5:0.03
Combine 950 mL HPLC grade methanol and 50 mL deionized water. Mix

well and
vacuum filter through a 0.5 pm PTFE membrane. Add 0.3 mL concentrated
ammonium
This is an unco.ntrolled copy of a controlled document.
a-,/ UYG
FBI Laboratory
Chemistry Unit
Toxicology Subunit
Issue
Tox I 03-2.doc
Date: 10/27/2006
Revision. 2
page 8 of 15
hydroxide and mix gently.

month.
dd.
Veriff pH>8. Store in glass at room temperature. Stable
LC Mobile Phase - Alkaline#2 (5:95:0.03 methanol:water:ammonia):

Combine 25 mL HPLC grade methanoland 475 mL deionized water. Mix well and
vacuum filter through a 0.5 pm PTFE membrane. Add 0.15 mL concentrated ammonium
hydroxide and mix gently. Verif, pH>8. Store in glass at room temperature. Stable
I
month.
LC Mobile Phase - Benzodiazepines (60 :40 :0.03 methanol:water:ammonia):

Combine 300 mL HPLC grade methanol and 200 mL deionized water. Mix well and
vacuum filter through a 0.5 pm PTFE membrane. Add 0.15 mL concentrated ammonium
hydroxide and mix gently. Verifu pH>8. Store in glass at room temperature. Stable I
month.
ff.
LC Mobile Phase - Rodenticide #l (0.1% acetic acid in water):

Vacuum filter 500 mL deionized water through a 0.5 pm PTFE membrane. Add 0.5 mL
ACS grade glacial acetic acid. Store in glass at room temperature. Stable I month.
go
LC Mobile Phase - Rodenticide #2 (0.1% acetic acid in methanol):

Vacuum filter 500 mL Optima grade methanol. Add 0.5 mL ACS grade glacial acetic acid.
Vacuum filter through a 0.5 pm PTFE membrane. Store in glass at room temperature.
Stable I month.
EE'
hh.
LC Mobile Phase
Mivacurium
#l
(acetonitrile):
Measure out 1000 mL HPLC grade acetonitrile and vacuum filter through a 0.5 pm pTFE
membrane. Store in glass at room temperature. Stable 2 months.
ll.
LC Mobile Phase - Mivacurium#Z (5 mM octanesulfonic acid):

Quantitatively transfer the contents of one vial of PICB-8 reagent into a 1000-mL
volumetric flask and bring to the mark with deionized water. Vacuum filter through a 0.5
pm PTFE membrane. Store in glass at room temperature. stable I month.
jj.
LC Mobile Phase - Mivacurium MSMS (40 60 :0.0 I 5 acetonitrile:water:methanesulfonic

acid):
Combine 200 mL HPLC grade acetonitrile, 300 mL deionized water, and 75 pl pIC reagent.
vacuum filter through a 0.5 pm PTFE membrane, and verifu 2<pH<3.5. Store at room
temperature in brown glass. Stable I month.
kk.
LC Mobile Phase - Succinylmonocholine #l (92:8:0.1 water:methanol:pIC reagent):

Combine 460 mL deionized water, 40 mL HPLC methanol, and 0.5 mL pIC
tuti*
well and vacuum filter through a 0.5 pm PTFE membrane. Store ar room remperature in
brown glass. Stable for I month.
..["ni.
Zr 4t/u
FBI Laboratory
t"-':j,'"H'H#lll
Issue
Tox 103-2.doc
Date: 10/27/2006
Revision: 2
Page9ofl5
ll.
LC Mobile Phase- Succinylmonocholine #z(80:15:4.75:0.25 0.1% HFBA:g.1 M

ammonium acetate:acetonihile: isopropanol) r
Combine 400 mL 0.1% heptafluorobutyric acid,75 mL 0.1 M ammonium acetate,23.75
mL HPLC grade acetonitrile, and 1.25 mL HPLC grade isopropanol. Mix well and
vacuum filter through a 0.5 pm PTFE membrane. Store in glass at room temperature.
Stable I month.
mm. l:l
Methanol:Dilule Hydrochloric Acid:
Combine 2 mL GC'grade methanol with 2 mL I M hydrochloric acid, and mix

in glass at room temperature. To be prepared fresh.
nn.
Combine 95 mL HPLC grade methanol with 5 mL deionized water and mix
well.
well.
Store in elass
Nitric Acid, Dilute (33%by volume):

Mix 5 mL concentrated nitric acid with 10 mL deionized water and shake to combine.
Store in glass at room temperature. Stable
qq.
Store in
l:l Methanol:Water:
Combine 50 mL HPLC methanolwith 50 mL deionized water and mix
at room temperature. Stable 6 months.
pp.
Store
95:5 Methanol:Water:
glass at room temperature. Stable 6 months.
oo.
well.
year.
0.2% (by volume) Nitric Acid:

To a 1000-mL Nalgene volumetric flask containing 600 mL deionized water, add 2 mL
Optima grade concentrated nitric acid. Bring to volume with deionized water and mix well.
Store in plastic at room temperature. Stable I year.
Extraction Solvent (90 : I 0 chloroform isopropanol) :

Combine 50 mL HPLC grade isopropanol and 450 mL HPLC grade chloroform and mix
well. Store at room temperature in brown glass. Stable I month.
Op iates
Palladium / Magnesium Nitrate Matrix Modifier for AAS (Atomic Absorption

Spectroscopy):
To a 100-mL Nalgene volumetric flask containing 50 mL deionized water, add l5 mg

magnesium nitrate and25 mL palladium matrix modifier solution. Bring to volume with
deionized water and mix well. Store at room temperature in Nalgene container. Stable 5
years.
Z^z
4+t,
.c
FBI Labomtory
Chemistry Unir
Toxicology Subunit
Tox I 03-2.doc
Issue
Date:
ljVD006
Revision: 2
Page
l0 of
I5
tt.
I 1.8 M Potassium Hydroxide:

To a 100-mLNalgene volumetric flask add 66 g potassium hydroxide and 50 mL deionized
water. Mix well to dissolve and bring to volume with deionized water. Store at room
temperature in Nalgene container. Stable I year.
uu.
5% (wlv) Potassium Phosphate Buffer (pH 4.5):

To a 100-mL volumetric flask, add 80 mL deionized water. Add 5 g monobasic potassium
phosphate and mix wellto dissolve. Bring to volume with deionized water, and veri$r
4.0<pH<5.0. Store refrigerated in glass. Stable I month.
vv.
l0% (w/v) Silver Nitrate Solution:

Dissolve 2 g silver nitrate in 20 mL deionized water. Store at room temperature in an
opaque container. Stable I year.
ww.
0.1
M Sodium Acetate Buffer (pH 7):
To a 250-mL volumetric flask, add 3.4 g sodium acetate trihydrate and 200 mL deionized
water. Mix well and adjust to 6.5<pH<7.5 by slow addition of I N hydrochloric acid.
Bring to volume with deionized water. Store refrigerated in glass. Stable 2 months.
xx.
Sodium Acetate Buffer with 5% Methanol:

Add 5 mL HPLC grade methanolto a 100-mL volumetric flask and bring to volume with
0.1 M sodium acetate buffer (pH 7). Store refrigerated in glass. Stable 2 months.
yy.
1.1 M Sodium Acetate Buffer (pH 5.5):

To a 100-mL volumetric flask, add 14.95 g sodium acetate trihydrate, 60 mL deionized
water, and2.2 mL glacial acetic acid. Mix wellto dissolve, and bring to volume with
deionized water. Verif 5<pH<6. Store refrigerated in glass. Stable 2 months.
zz.
0.1 M Sodium Borate Buffer (pH 9):

To a 100-mL volumetric flask add 3.8 g sodium borate and bring to volume with deionized
water. Sonicate for l5 minutes to assist dissolution, and verifu 8.5<pH<9.5. Store
refrigerated in glass. Stable 3 months.
aaa.
Saturated Sodium Chloride Solution (- 35%wlv):

To a 500-mL volumetric flask, add 450 mL deionized water and 175 g sodium chloride.
Gently heat with continuous stining for at least one hour. Remove the stirbar, fill to
volume with deionized water, and mix by inversion. A small amount of undissolved solid
should remain in the bottom of the flask. Store in glass at room temperature. Stable for
one year.
5"
uvL,
:i::t'ffi#
'*1*?,*o:::
Issue
Date: 10/27/2006
Revision: 2
Page
of15
ll
bbb.
0.287 M Sodium Dithionite Reducing Agent:
To a 50-mL volumetric flask, add 40 mL deionized water and 236 gsodium dithionite.
Mix well to dissolve and bring to volume with deionizedwater. Store in glass at room
temperature. Stable I month.
ccc.
ddd.
0.1 M Sodium Hydroxide:

To a 100-mL Nalgene volumetric flask, add 60 mL water and 0.4 g sodium hydroxide.
Mix
well to dissolve and bring to volume with deionized water. Store in Nalgene containers at
room temperature. Stable 1 year.
5
M (20% w/v) Sodium Hydroxide:
To a 100-mL Nalgenb volumetric flask, add 60 mL water and 20 g sodium hydroxide. Mix
well to dissolve and bring to volume with deionized water. Store in Nalgene containers at
eee.
0.1 M Sodium Phosphate Bufler (pH 6.0):

To a 500-mL volumetric flask, add 400 mL deionized water, 6.1 g sodium phosphate
monobasic monohydrate, and 1.6 g sodium phosphate dibasic heptahydrate. tvti* well to
dissolve. Verifr 5.8<pH<6.1, adjusting pH by addition of 0.1 M dibasic sodium phosphate
(increases pH) or 0.1 M monobasic sodium phosphate (decreases pH) as necessary. Bring
to volume with deionized water. Store refrigerated in glass. Stable I month.
fff.
0.1 M Sodium Phosphate, Dibasic:
To a 100-mL volumetric flask, add 2.7 g sodium phosphate dibasic heptahydrate and 80
mL deionized water. Mix wellto dissolve and bring to volume with deionized water.
Store refrigerated in glass. Stable I month.
goo
0.1 M Sodium Phosphate, Monobasic:

To a 100-mL volumetric flask, add 1.4 g sodium phosphate monobasic monohydrate and
80 mL deionized water. Mix well to dissolve and bring to volume with deionized warer.
Store refrigerated in glass. Stable I month.
hhh.
SPE (Solid Phase Extraction) Alkaline / Cocaine Elution Solvent (78:20:2 methylene
chloride : isopropanol : ammonia) :
Combine 20 mL HPLC grade isopropanolwith 2 mL concentrated ammonium hydroxide

and mix well. Add 78 mL HPLC grade methylene chloride and mix well. Store in
slass at
room temperature. To be prepared fresh.
lll.
SPE Benzodiazepines Elution Solvent (49:l ethyl acetate:ammonia):

Combine 49 mL ethylacetate with I mL concentrated ammonium hydroxide and mix well.
Store in glass at room temperature. To be prepared fresh.
{4
'1'4r*,
/\
/ it<\
i?::t'ffl,'#
Toxicology Subunit
trrr.o.J:lJr?;ff;
Revision: 2
Page
jjj.
kkk.
ll
l.
l2ofl5
SPE Benzodiazepines Wash Solvent (20% acetonitrile in 0.1 M phosphate buffer):

Combine 80 mL 0.1 M phosphate buffer (pH 6) with 20 mL HPLC grade acetonitrile and
mix well. Store in glass at room temperature. Stable I month.
SPE THC Elution Solvent aka Rodenticide Wash Solvent (95:5 hexane:ethyl acetate):
Combine 95 mL hexane with 5 mL ethyl acetate and mix well. Store in glass at room
sPE THC-cooH Elution Solvent aka Rodenticide Elution Solvent (75.25:l hexane:ethyl
acetate:acetic acid):
Combine 75 mL hexane with 25 mL ethyl acetate and I mL glacial acetic acid. Mix well.
Store in glass at room temperature. Stable I month.
mmm.5NSulfuricAcid:
To a 100-mL graduated cylinder containing 70 mL deionized water, slowly add 12.5 mL
concentrated sulfuric acid. Mix well and bring to 90 mL with deionized water. Store in
glass at room temperature. Stable I year.
nnn.
5% (by volume) Sulfuric Acid:

To a 100-mL volumetric flask containing 80 mL deionized water, slowly add 5 mL
concentrated sulfuric acid. Mix well and bring to volume with deionized water. Store in
glass at room temperature. Stable I year.
ooo. I M Sulfuric Acid with I .5% (wlv) Saponin:

Add 80 mL deionized water and 1.35 g saponin to a 100-mL graduated cylinder and mix
well to dissolve. Slowly add 5 mL concentrated sulfuric acid. Bring to the 90-mL mark
with deionized water and mix well. Store in glass at room temperature. Stable I year.
ppp.
THC-COOH Extraction Solvent (7:l hexane:ethyl acetate):

Combine 70 mL hexane with 10 mL ethyl acetate and mix well. Store in glass at room
qqq.
TMAH Reagent:
Dissolve 0.25 gtetramethylammoniumhydroxide in I mL deionized water. Add 20 mL
dimethylsulfoxide and mix well. Store refrigerated in brown glass. Stable I year.
rrr.
0.04% (by volume) Trifluoroacetic Acid (TFA):

To a 100-mL volumetric flask, add 90 mL deionized water and 40 pltrifluoroacetic acid,
Mix well and bring to volume with deionized water. Store in glass at room temperature.
Stable 3 months.
This is an uncontrolled copy
o)t
contrTlled document.
J'u
4L,
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FBI Laboratory
Chemrstry Unit
Toxicology Subunit
Tox I 03-2.doc
Issue
Date:
1012712006
Revision: 2
Page l3 of l5
sss.
Trinder'sReagent:
Add 400 mg mercuric chloride, 400 mg fenic nitrate nonahydrate , and 0.1 mL
concentrated hydrochloric acid to 5 mL deionized water in a 10-mL volumetric flask. Mix
well to dissolve and bring to volume with deionized water. Store refrigerated in glass.
Stable 6 months.
Not applicable.
Decision Criteria
Not applicable.
9 Calculations
Not applicable.
Not applicable.
11 Limitations
Not applicable.
12 Safety
Follow standard precautions for the handling of chemicals and biological materials. Refer to the
FBI Laboratory Safety Manual for guidance.
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Issue Dare: 10/2712006
Revision: 2
Page
l4 of
13 References
Shugar, G. J.; Ballinger, J.T. Chemical Technicians' Ready Reference Handbook, 3'd
Ed;
McGraw-Hill: New York. NY. 1990.

FBI Laboratory Safety Manuol,
Toxicologt Subunit SOP Manual.
Chemistry Unit Procedurefor Verification of Reagents, Kits, Solvents and Standards (CUQA 9);
FBI Laboratory Chemistry Unit Quality Assurance Manual.
i-v
44 G
FBI Laborarory
Chcrnistry Unit
'I'oxicology
Subunit
Issue
l'ox l0!2,doc
Daie; l0lZ712006
Rcvision:
pagc
Rev.
#
0
L
Date
l/30/06
New document.
6121106
Added new reagent (saturated sodium chroride), and removed
Issue
History
%
several (insulin ELISA reagents).
tat27/a6
Apnroval
Chemistry Unit
Added new reagents (mobile phases for rodenticides).
; A
//l
Chief: ' I/UUW
n
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Date:
Marc A. LeBeau
OA Apnroval
Qualiry Manager:
Issuance
Tox Subunit Manager:
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FBI Labontory
Chemistry Unit
Toxicology Subunit
Tox I 04-0.doc
Revision: 0
Page
I of
15
Guidelines for Comparison of Mass Spectra
Introduction
Many of the analytical procedures used in the Toxicology Subunit rely on mass
spectrometry to
help establish identification of individual chemical entitils within a sample.
In oider to ensure
consistency and reproducibility in compound identification, it is desirabie
to have guidelines for
the comparison of known and unknown mass spectra.
2 Scope
This
document provides guidelines to help determine what constitutes a match between

known
and unknown mass spectra. Various critical characteristics of a mass spectrum
are defined, and
procedures for using these characteristics to evaluate matching between
spectra are laid out. Note
that this document provides guidelines for the matching of miss spectra, and
does not directly
address compound identification. A good quality masJspectral match will normally
be onlytne
element in establishing the identity of an unknown substance. These protocols are intended
for
application to full scan, tandem, and selected ion monitoring (SIM) mass spectra acquired
in
electron impact (EI), chemical (CI), electrospray (ESI), and atmospheric piessure chemical
ionization (APCI) modes. other mass spectral techniques are beyond the scope of this
document.
3 Principle
The spectrum of a given unknown of interest is compared to the known spectrum of
a target
analyte. The unknown spectrum should contain all the significant ions present in the
known
spectrum, and should not contain any unexplained significant ions not seen in the known
spectrum.
The relative intensities (hereafter referred to as "ion ratios") of several selected characteristic
ions
should match in both spectra, to within defined tolerances. These guidelines draw heavily
on
technical document 2003IDCR from the World Anti-Doping Agency, the 2003 recommendations
of the American Society for Mass Spectrometry's Measur.r.nts and Standards Committee,
and
the2002 National Committee for Clinical Laboratory Standards Approved Guideline
for GC/Tr4S
(gas chromatography/mass spectrometry) Confirmation of Drugs.
4 Specimens
Not applicable.
5 Equipment/Materials/Reagents
{u +v t/::;,,\
FBI Laboratory
Chemistry Unit
Toxicology Subunit
Tox 104-0.doc
lssue Date: 06/21106
Revision: 0
Page2ofl5
Not applicable.

Not applicable.
7 Calibration
The calibration of all mass spectrometers should be verified regularly per the appropriate
instrument protocols inthe Instrument Operations and Support Subunit SOP Manual.
8 Sampling
Not applicable.
9 Procedure
Provided below are procedures for defining and determining critical characteristics of a mass
spectrum to be used in establishing whether or not two spectra match. An abbreviated list of the
key points is provided in Appendix L
9.1 Averaging and Background Subtraction of Mass Spectra

In many real-world samples, it may be necessary to correct mass spectra of interest for the
presence of ions resulting from sample background, instrument background, or partially coeluting
sample components. The necessary background-subtracted spectrum will usually be generated by
averaging not more than five spectra across the peak of interest and then subtracting the average
of a number of background spectra equalto not more than twice the number of sample spectra. The
background spectra may come before and/or after the sample spectra, and should all be selected
from outside the region integrated for determination of ion ratios. This background-subhacted
spectrum will be used to establish the list of significant ions and the base peak for that spectrum.
9.2 Determination of "Significant lons" in
a Mass Spectrum
Any ion signal greater than l5% of the most intense ion signal in a background-subtracted mass
spectrum will normally be considered a signiJicant ion. An ion that would otherwise be
considered significant may be excluded if it can be demonstrated that the ion arises from, or is
significantly disturbed by, an uncorrectable chemical interference. Such interferences will
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normally be demonstrated by showing that a reconstructed ion trace for the ion in question is not
coincident with the traces for other ions associated with the component of interest.
9.3 Determination of "Diagnostic Ions" in a Mass Spectrum

Diagnostic ions are those ions in a mass spectrum that are characteristic of the chemical
compound under investigation. Determination of diagnostic ions depends upon knowledge of the
chemical structure of a component under investigation, and may therefore only be determined
from mass spectra of known standards. The definition of what makes any given ion
"characteristic" of a particular chemical structure is somewhat nebulous, and there does not appear
to be any universally accepted standard in the field. This means that good and consistent judgment
by the examiner is essential. There are, however, recommendations as to what renders some ions
nonspecific and not diagnostic, and an examiner should abide by these practices when eliminating
ions from consideration as diagnostic.
Adduct ions will normally be excluded, except that one pseudomolecular adduct ion may be
considered diagnostic. Isotopomers will be excluded unless they are characteristic of a specific
chemical composition. Normally this will be limited to chlorine and bromine isotopomers, but
other possibilities may arise. Ions resulting purely from a derivatizing or complexing reagent will
normally be excluded from the list of diagnostic ions. For example,themlz 73 ion of a
trimethylsilyl derivative may not be chosen as a diagnostic ion. Normally the (pseudo)molecular
ion for a compound will be considered diagnostic, unless the intensity for that ion is less than 5%o
of the intensity for the base peak in the background-subtracted spectrum of the component in
question.
9.4 Determination of the "Base Peak" in a Mass Spectrum

The base peak for the mass spectrum of a known standard is the most intense signal for a
diagnostic ion in the background-subtracted spectrum. For the purpose of determining relative ion
intensities the base peak in an unknown mass spectrum will be taken as the base peak of the
standard spectrum to which it is being compared, even if a different diagnostic ion shows higher
intensity in that spectrum.
In instances where it can be demonstrated that the nominal base peak signal is significantly
disturbed by an uncorrectable chemical interference, the second most intense diagnostic ion
present in the spectrum may be used as the base peak. Such interference will normally be
demonstrated by showing that a reconstructed ion trace for the ion in question is not coincident
with the traces for other ions associated with the component of interest.
9.5 Method for Calculating Ion Ratios

Ion ratios will normally be determined by integrating reconstructed ion traces for each diagnostic
ion present in a given component. All integrations of reconstructed ion traces from a given
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lssue Date: 06121106
Revision: 0
Page 4
of l5
component should have comparable stop and start points. Ion ratios are then calculated by
dividing the area for each ion trace by the area for the trace ofthe base peak ion, and expressing the
result as a percentage. In instances where the reconstructed ion traces produce non-integratable
data, it is acceptable to substitute ion abundances from the background subtracted spectrum of the
compound of interest for the integrated areas from reconstructed ion traces. This will normally
happen in situations where multiple sorts of mass spectral data are simultaneously acquired in a
single analytical run, resulting in discontinuous data streams for the various individual mass
spectral experiments.
l0
Instrument Conditions
Not applicable.
1l Decision Criteria
Provided below are guidelines for establishing a match between a known mass spectrum and that
of an unknown spectrum. Note that some analytical standard operating procedures (SOP's)
include detailed criteria for the evaluation of mass spectra of individual target analyes. Such
specific instructions will supercede the guidelines provided below.
In almost all cases, unknown spectra should be matched against known spectra obtained from
contemporaneously analyzed reference material. Exceptions are discussed in section 12.5 of these
guidelines. When assessing spectra for a targeted analyte from multiple unknown samples in a
single analytical run, it is acceptable to compare each unknown spectrum to the known spectrum
resulting from a different contemporaneously analyzed reference sample. The mass spectra of
many chemical entities are known to vary with analyte load. It is acceptable to dilute and
reanalyze a sample containing a high level of a suspected target compound in order to be able to
more appropriately match its spectrum to a lower concentration standard, control, or calibrator.
11.1 For Full Scan Mass Spectra

In order to establish a match between known and unknown mass spectra in the full scan mode, both
of the followine criteria should be met:
Every significant ion present in the known spectrum should be present in the unknown
spectrum, and vice-versa.
b.
All
relative intensities for diagnostic ions in the unknown spectrum should match those
observed in the known spectrum within the tolerances shown in Table I or Table 2.
these limits would produce an acceptable lower bound of less than lo/o for a given ion ratio,
If
This is an uncontrolled copy of a controlled document,
Z'w/\ qq U
1O,s3)
FBI Laboratory
Chemistry Unit
Toxicology Subunit
Tox 104-0.doc
Revision: 0
Page 5
of
15
will be set at 106. Ion ratios for specific diagnostic ions may be excluded
from consideration if they meet any of the following criteria:
the lower limit
l.
2.
J.
The ion ratio for that ion in the known spectrum is less than 5o/o (less than l\Yo for
CI, ESI, or APCI spectra).
The signal-to-noise ratio of the reconstructed ion trace for that ion in the unknown
spectrum is less than 3.
It can be shown that the signal for that ion in either the known or the unknown
spectrum is significantly disturbed by an uncorrectable chemical interference.
Such interference will normally be demonstrated by showing that a reconstructed
ion trace for the ion in question is not coincident with the traces for other ions
associated with the component of interest.
If there
are more than four diagnostic ions in the known spectrum, then the examiner need only
evaluate the ratios for four diagnostic ions (three ratios) in order to establish a scientifically valid
match between the spectra. For compounds with a molecular weight less than 80 AMU, only three
diagnostic ions (2 ratios) need be evaluated to establish a scientifically valid match. The selected
ions will normally include the base peak and the (pseudo)molecular ion, unless those ions meet
one ofthe three exclusion criteria given above. If fewer than three diagnostic ions are available for
evaluation, the specha may still be matched, but the examiner should be aware that the information
content derived from such a match is limited, and should be regarded with caution. Examiners
should also take care to ensure that the chosen scan range provides adequate "buffer space" around
the diagnostic and significant ions of the substance in question.
l:
Ion Ratio Matching 'l'olerances tor El Mass

Table
>5IYo
If the ion ratio in the known
spectrum is:
Then the ion ratio in the unknown
sDectrum should be
able
l0% absolute
>25o and <50%

20%o
relative
<2504
5% absolute
within:
7: lon Ratto Matchiln Tol erances for CI.
If the ion ratio in the known

snectrum is:
Then the ion ratio in the unknown
snectrum should be within:
APCI M ASS
ESI. and
a
>60Vo
l5% absolute
>40Yo and <60%o

25Vo
rclative
<40%
10% absolute
11.2 For SIM Mass Spectra

Selected ion monitoring experiments can allow for the detection of very low levels of analyte in
complex sample matrices, at the cost of reducing the information content of that experiment.
Examiners should take great care in selecting monitored ions for a SIM experiment. Ions for a
SIM experiment must be based upon a known full scan spectrum of the species of interest collected
5, v4b
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'*'Tii?Jll:::
Revision: 0
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on the instrument to be used for the SIM experiment. Four diagnostic ions will normally be
selected (three ions for compounds with a molecular weight less than 80 AMU; see 12.4 for
another exception), and, if possible, all should be significant as well as diagnostic. The base peak
be one of the chosen ions, and the (pseudo)molecular ion should be included if it has
a relative intensity greater than 5o/o in the known full scan spectrum. In order to establish a match
between a known SIM spectrum and an unknown SIM spectrum, all resulting ion ratios should
meet the tolerances specified in Table I or Table 2, as appropriate.
will normally
11.3 For Tandem Mass Spectrometry (MS/LS)

Tandem mass spectrometry can lend a great deal of additional specificity to mass spectral
experiments by greatly increasing the confidence that the ions in a given spectrum are all
associated with a single substance. Due to the nature of most collision-induced dissociation
processes, however, ion ratios in tandem mass spectra tend to be much less stable, and much more
dependent on analyte load, than is true for classic electron impact mass spectra,
Tandem mass spectra tend to be much "cleaner" than full scan mass spectra, with fewer extraneous
ions. Therefore, the limit for determination of significant ions in a tandem mass spectrum is
lowered to l}Yo (from l5%) of the most intense observed ion in the background subtracted
spectrum. The high probability of ion association in tandem mass spectrometry means that nearly
all ions of reasonable intensity observed in an MS/lvIS experiment should be considered diagnostic,
with the exception of ions resulting purely from the loss of an adduct.
Due to vagaries of the physical processes involved in the precursor ion isolation and fragmentation
events in an ion trap mass spectrometer, tandem mass spectra acquired on such an instrument will
occasionally show an "ion-splitting" artifact for a precursor ion returned in a product ion mass
spectrum. This is evidenced by the presence of trvo ions, separated by a fraction of an AMU, at the
nominal mass of the precursor ion in the product ion spectrum. In instances where this
phenomenon is observed, the response for the affected ion should be taken as the total of the
response for both components of the "split" ion signal.
11.3.1 Product Ion Experiments

When conducting product ion experiments, the selection of a precursor ion is critical to obtaining
useful and reliable information. In most cases, the (pseudo)molecular ion of the species under
consideration should be selected, if available. It is also acceptable to use a diagnostic isotopomer
of the (pseudo)molecular ion, if one is available. If the (pseudo)molecular ion is not available, or
is not suitable for some reason, then the selected precursor ion should be both significant and
diagnostic in the full scan mass spectrum of the substance under consideration. With product ion
spectra, it is also important to ensure that the observed fragment spectrum is, in fact, emerging
from the selected precursor ion. For this reason, one of the fwo following criteria should normally
be met for a product ion spectrum:
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a.
The precursor ion should be observed in the product ion spectrum with an ion ratio of at
least 5%.
b.
scan mass spectral data are collected concunently with the product ion spectra, the
scan spectrum of the component of interest should show no ions within 1.5 AMU of the
If full
full
precursor ion with greater than three times the intensity of the precursor ion.
In order to establish a match between a known product ion spectrum and the product ion spectrum
of an unknown, both of the following criteria should be met:
a.
b.
Every significant ion present in the known spectrum should be present in the unknown
spectrum, and vice-versa.
All relative intensities for diagnostic ions in the unknown spectrum should match those
observed in the known spectrum to within the tolerances shown in Table 3. If these limits
would produce an acceptable lower bound of less than loh for a given ion ratio, the lower
Iimit will be set at0.5o/o. Ion ratios for specific diagnostic ions may be excluded from
consideration if they meet any of the following criteria:
1.
2.
3.
The ion ratio for that ion in the known spectrum is less than 5%a.
The signal-to-noise ratio of the reconstructed ion trace for that ion in the unknown
spectrum is less than 3.
It can be shown that the signal for that ion in either the known or the unknown
spectrum is significantly disturbed by an uncorrectable chemical interference.
Such interference will normally be demonstrated by showing that a reconstructed
ion trace for the ion in question is not coincident with the traces for other ions
associated with the component of interest.
are more than three diagnostic ions in the known spectrum, then the examiner need only
evaluate the ratios for three diagnostic ions (two ratios) in order to establish a scientifically valid
match between the spectra. The selected three ions should include the base peak and the precursor
If there
ion (if present), unless those ions meet one of the three exclusion criteria given above. If only a
singie diagnostic ion is observed in the product ion spectrum, spectra may still be matched, but the
.*u*in.r thould be aware that the information content derived from such a match is limited, and
should be regarded with caution.
Table
MS/M5
for MS/lvlS
lor
ol
3: Ion Ratio Matchtng lolerances
Prod
Hrooucl Ion
>400
If the ion ratio in the known spectrum is:

Then the ion ratio in the unknown spectrum should be within:
25o/o
relative
E"
t/4 r-
/as,t,
s40%
l0% absolute
FBI Labordtory
Chemistry Unit
Toxicology Subunit
Tox 104-0.doc
Revisron: 0
Page 8
of
15
LL.3.2 Precursor Ion and Neutral Loss Experiments

The practical information content for precursor ion and neutral loss MS/lvIS experiments is
generally low, but circumstances may stillarise in which one of these techniques can provide
critical additional information about a given substance. For precursor ion experiments, a match
between a known and an unknown spectrum may be established if all significant ions present in
the known spectrum are present in the unknown spectrum, and vice-versa. For neutral loss
experiments, a match between a known and an unknown spectrum may be established if all
significant transition pairs present in the known spectrum are present in the unknown spectrum
and vice-versa.
11.3.3 Selected Reaction Monitoring (SRM) Experiments

SRM analysis shares many features, advantages, and limitations with SIM analysis, but benefits
from the added specificify afforded by tandem mass spectrometry. Three diagnostic ion
transitions should be chosen for an SRM experiment. Generally, all three transitions should share
a common precursor ion, although it is appropriate to use multiple precursor ions if all are part of
a diagnostic isotope cluster in the full scan spectrum of the substance in question. It is desirable
that the chosen precursor ion be the (pseudo)molecular ion of the substance in question. If this is
not possible, or not practical, then the chosen precursor ion should be both significant and
diagnostic in the full scan spectrum of the substance in question. In order to establish a match
between a known SRM spectrum and an unknown SRM spectrum, both resulting ion ratios should
meet the tolerances specified in Table 3'
11.3.4 Higher Order (MS") Tandem Mass Spectrometry

Tandem mass spectra of order higher than2 are beyond the scope of this document. There is little
to no discussion of this subject in the various published technical guidelines, and the technique is
rarely practiced in forensic and regulatory settings. When used, higher order tandem mass spectra
will be addressed on a case-by-case basis, usually as a part of method validation. Examiners
should consider using the criteria for product ion MS/MS in section 12.3.1 as a starting point for
such evaluation.
11.4 Exact (Precise) Mass Measurement Techniques

Exact mass measurement can provide a significant additional level of information content in a
mass spectrum, giving an examiner more confidence in any conclusions based upon that spectrum.
The use of exact mass measurement techniques does not, however, allow an examiner to disregard
other aspects of the mass spectrum under consideration. As such, mass spectra obtained using
exact mass techniques should still meet all of the matching criteria for the appropriate mass
spectral techniques given above, but different standards may be used in selecting diagnostic ions,
and more confidence can be placed in matches based upon a limited set of diagnostic ions.
This is an uncontrolled
co_py
of a controlled document.
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Revision: 0
Page9ofl5
Ions in an unknown spectrum willbe considered to be an exact mass match to those in a known
spectrum if the measured masses agree to within 0.005 AMU. For a SIM experiment, only three
ions, instead of four, need be monitored, and show appropriate ion ratio agreement, if all three ions
meet this exact mass match criterion. When determining diagnostic ions, any isotopomer of a
(pseudo)molecular ion may be considered diagnostic if it meets this exact mass match criterion.
One additional adduct ion, beyond the pseudomolecular ion, may also be considered diagnostic if
it meets this exact mass match criterion.
11.5 Matching to Library Spectra

While mass spectral libraries (either commercial compendia or collections generated in-house)
can be invaluable tools in helping to direct examinations and suggest possible targets for further
investigation, an examiner should remain aware of the limitations of these libraries, Most
commercial libraries do not clearly indicate the instrumentation the spectra were acquired on, or
at what level of sample loading. In-house library data may have been acquired on the same
instrumentation used to obtain a given unknown spectrum, but it is very difficult to ensure that
long-term drift in instrument performance has not compromised the reproducibility of those
library spectra.
Despite these limitations, there may arise rare instances in which it is necessary to compare an
unknown spectrum to a library entry, for example if a standard of the substance in question cannot
be readily obtained, or for purposes of screening to direct further investigation. In cases where
such matching is attempted, all criteria for the appropriate type of mass spectrometry, given above,
should still be observed, with one significant change. In these instances, ion abundances for the
determination of ion ratios will be measured as the intensity of the ion in the spectrum, rather than
as the integrated area of a reconstructed ion trace. For the unknown spectrum, all criteria
regarding averaging and background subtraction from section 10.1 should still be observed.
12 Calculations
IR*
(A*/A6)xl 00%, where:
IR* = the ion ratio for ion x

A* : the integrated area of the reconstructed ion trace for ion x
4,6: the integrated area of the reconstructed ion tpace for the base peak ion
(lon abundances from background subtracted mass spectra may be substituted for integrated areas
under certain circumstances detailed in section 9.5.)
Not applicable.
t*
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FBI Laboratory
Chemistry Unit
Toxicology Subunit
Tox I 04-0.doc
Revision: 0
Page
l0ofl5
14 Limitations
This procedure, while extensive, is not intended to be exhaustive, and situations will arise in which
their blind application could lead to inappropriate conclusions. No set of rules can ever replace the
good judgment of a trained and experienced examiner. The mere fact that an unknown mass
spectrum matches wellto the spectrum of a known standard will rarely, by itself, be sufficient
grounds to claim the presence of that compound in the questioned sample. All of the analytical
data for the samples in question should be considered when drawing such final conclusions.
Similarly, the fact that an unknown mass spectrum fails to match that of a known standard
generally will not, by itself, constitute grounds for concluding that the compound is not present in
the questioned specimen.
This protocol does not excuse an examiner from exercising care in the acquisition of mass spectral
data. It should be remembered that poor practices in the acquisition of mass spectra willyield data
that is useless at best, and misleading at worst. Samples that show evidence of severe
chromatographic overload should generally be diluted and reinjected in order to obtain reliable
mass spectra. Instrument calibration is also critical for obtaining useful mass spectral data, and it
is incumbent upon any examiner to run appropriate test samples to demonstrate proper instrument
function.
15 Safety
Not applicable.
16 References
Betham, R.,; Boison, J.; et al J. Am. Soc. Mass Spectrom.2003,14,528-541.
deZeeuw, R. A.
Forensic Sci. 2005, 50,745-747.
Mclafferty, F. W.; Stauffer,
Soc. Mass Spectrom. 1999,
10. t229-1240.
A. Forensic Sci. Int. 2004. 145.85-96.
deZeeuw, R. A. -r. Chrom. B 2004,811, 3-12.
Technical Document TD2003IDCR, 2004; World Anti-Doping Agency, Montreal, Canada.
Bowers, L. D.; Armbruster, D.A.; et aINCCLS DocumentC43-A,2002:The NationalCommittee
Ev ?ub
(at'\
FBI Laboratory
Chemistry Unit
Toxicology Subunit
Tox I 04-0.doc
lssue Date: 06/21/06
Revision: 0
Page
for Clinical Laboratory Standards, Wayne, PA.

Instrument Operations and Support Subunit SOP Manual,
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of15
liBl l.aboratorr
Chemistry Lrrrit
Toxicology Suhunir
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0621n6
Issue
History
Original Issue
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Quality ivlanager:
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Appendix
l.
l:
Mass Spectra Key Points
AveraginglBackground Subtraction of Mass Spectra: (* = subtracted spectrum)

<6 scans averaged for sample (N)
a.
b.
c.
<2N+l
scans for background
background outside area integrated for ion ratios
2.
Significant Ions: Ion signal >
3.
Diagnostic Ions (determine from mass spectra of known standard):

Characteristic of chemical compounds chemical structure
Diagnostic criteria (not well defined):
(Pseudo)molecular ion is diagnostic if intensity > 5% base peak
Non-diagnostic ions (generally exclude):
Adduct ions except pseudomolecular ion
Isotopomers except chlorine and bromine isotopomers
Ions 2nory to a derivatizing reagent (e.g. m/z 73 TMS deriv)
l5o
(10% for MSA4S) of most intense ion signal
(*)
a.
b.
c.
(*)
4.
Base Peak (determined from mass spectra of known standard):

Most intense signal for diagnostic ion (*)
Base peak standard is base peak unknown (Exception: can use second most intense
diagnostic ion if base peak has an uncorrectable chemical interference)
5.
Method for calculating relative ion intensities:

Determine ion abundances = integrate RIC's / EIC's for each diagnostic ion
Integration - comparable stop & start points
Ion ratios (expressed as o/o) = each ion trace area/base peak ion area
Spectral peak height may be substituted for integrated area if the RIC data in
non-integrable.
a.
b.
a.
b.
c.
d.
6.
Decision Criteria: Unknown spectra matched against known spectra.
6.1
Full Scan Mass Spectra

Every significant ion in known spectra present in unknown and vice-versa
Relative ion intensities (EI)
Known Ion ratio > 50yo - unknown l0% absolute
Known Ion ratio 25-50% - unknown 20%orelative
Known Ion ratio <25yo - unknown 5% absolute
c. Relative ion intensities (CI, ESI, APCI)
Known Ion ratio > 600A - unknown 15% absolute
Known Ion ratio 40-60% - unknown 25Yorelative
Known Ion ratio < 40Vo - unknown 10% absolute
a.
b.
5"
l
q+b
r'e)
ii:*t'tr;"#
'*'Ti:?oi:oo:::
Revision: 0
Page 14 of I 5
6.2
SIM Mass Spectra

a. Four diagnostic ions (three for compounds <80 AMU), all should be significant
b. Base peak one ofthe chosen ions
c. (Pseudo)molecular ion RI > 5%
d. Meet relative ion intensities
6.3
Tandem MS (ion ratio dependant on analyte load, less stable)

All ions of reasonable intensity are diagnostic (Exception 2ndv loss of adduct)
6.3.I
Product Ion (Daughter Ion) Experiment

Select precursor ion (parent ion):
(Pseudo)molecular ion or one of its isotopomers
Product spectra:
Precursor ion observed with ion ratio >5% OR full scan show no ions
within 1.5 AMU of precursor ion with > 3x intensity of the precursor ion
Comparing product spectra (Standard to unknown = std to unk)
Significant ions present both std and unk
If > 3 diag ions -need only ratio 3 diag (2 ratios)
Ion ratios:
Known > 40yo - unknown 25%o relative
Known < 40Yo - unknown l0% absolute
Exclude ion ratios if:
Ion ratio known < 5olo
Signal-to-noise RIC unknown < 3
Chemical interference in ion
a.
a.
b.
c.
6.3.2
Precursor ion and Neutral loss
6.3.3
Selected Reaction Monitoring

3 diagnostic ion transitions
Share common precursor ion, except isotopomer clusters
6.4
a.
b.
c.
must match stds with unknowns
Ion ratios:
Known > 40yo - unknown 25%orelative
Known < 40o - unknown l0% absolute
Exact Mass (Accurate Mass)

rn/z < 600: Std to Unk measured masses within 3 mAMU
m/z> 600: Std to Unk measured masses within 5ppm
SIM: only 3 ions need monitoring, in correct ratios
a.
b.
c.
d.
If
above criteria is met:

Can use (pseudo)molecular ion if < 5% zu
Can use any isotopomer of (pseudo)molecular ion
f*
qvL,
(-r,;\
'
FBI Laboratory
'",.'!i,"?)'flJlil
Tox 104-0.doc
'#l!'lii3
can use up to one additional adduct ion, beyond pseudomorecular ion
Appendix 2: Glossary of Terms
Adduct Ion - Any ion to which another chemical entity has been attached by a means other than
covalent bonding.
Base Peak
The most intense or abundant diagnostic ion in the mass spectrum of a substance.
Diagnostic Ion - Any ion observed in the mass spectrum of a substance that is characteristic of the
chemical structure of that substance.
Ion Ratio
The relative abundance or intensity of t'wo ion signals in a mass spectrum.
Isotopomers - Two or more chemical species that differ only in isotopic composition. For
example, CH3OH and CD3OH are two isotopomers of methanol.
Molecular Ion - A charged intact molecular species, with charge acquired solely through the gain
or loss of electrons. Normally denoted as M* or M- for singly charged species.
Precursor Ion
In tandem mass spectrometry, the ion selected for fragmentation. Often refened
to as a "parent ion",
Product Ion
In tandem mass spectrometry, an ion resulting from the fragmentation of another ion.
Often refened to as a "daughter ion".
Pseudomolecular Ion - A charged molecule in which charge has been acquired through adduction
of an ion or through loss of a moiety able to dissociate in solution. Examples include (M+H)*,
(M-H)-, (M+Na)*, and (M+NHa)+.
- A display of the abundance or intensity of a single ion signal as a

function of time during an analysis. Often also called an "extracted ion chromatogram" (EIC) or
"reconstructed ion chromatogram" (RIC).
Reconstructed Ion Trace
Significant Ion
- Any ion in the mass spectrum
of a substance present above a specified intensity
or abundance.
8y qqL,
(;
VALIDATION
iio +4+.
Gr)
Chemistry Unit
Method Validation Review Form
ProcedureName:
Arur,ysrs o7 EwA
nt Dprrn Fuoogrr^,n,
tr
Measurement of PhysicaUChemical Property
p/
nstablishment of Presence/Absence of Specific Analyte(s)/Class(es)
tr
Quantitation of Specified Analyte(s)
g/
Selectivtty: Analysis of at least l0 sources ofblank

matrix + 2 zero samples (blank matrix spiked with
internal standard). Analysis of samples spiked with
other compounds expected to be in real samples.
Calibration Model Qinearity)..Analysis of at least

non-zero calibrators at a minimum of 5 replicates
per level,
5
Bias, Repeatability, and Intermediate Precision:

QC samples at low and high conc in calibration
range. Analysis ofduplicates ofeach conc in at least
5 runs,
Limit of Detectioz;
See
Procedure for details.
tr
lpwer Limit of Quantitation:
g/
UooX t6rcts.'For LC-MS(-MS) procedures only.
See Procedure
for
details.
Analysis
of5
zltLldt,
zlBloz
neat standards and 5 blank extracts
Additional Comments:
This method has been appropriately validated for its intended use (as specified above). The method is considered fit for the
above use.
lt
Date: 7/l'' / 07
Unit Chief Approval:
fi
vuu
ftoa)
METHOD
{^r V4Lr
(^rr)
Instrument Method:
EDTA
pos Swabs.meth
LCQ
fnstrument Method
Creator: Adminislrator
Last modified: 2/12/OZ by Administrator
MS Run
Time (min) : L0.00
Divert Valve: not used during run

MS
Detector Settinqs:
Segment l_
fnformation
Duration (min) :
l_0. 00
Number of Scan Events: l_

Tune Method: EDTA_pos_CID
Scan Event
1:
Details:
. (293.0)->o(fZS.O-3j_5.0)
MS/MS: CE 15. 0? IsoW l_.0
Pos
Monday, February
12,
2OO7
12:55:05
{-v q4 c.
page
1 of
InsLrument Method:
EDTA
pos Swabs.meth
Waters 2690 LC Systern
Syringe draw rate (pl/sec) :2.50
Injection volume (UI) :5
settings:.
Solvent A:5:95 ACN:Water
Solvent B:B
Solwent C:C
Sol-vent D: D
Min pressure (pSI):0
Max pressure (PSf) :5000
Chart output: Pressure
Chart output:Normal
Pump
Gradient program:
Time (min)
Flow (nl/min)
0. 00
3. 00
0.30
0.30
0.06t
NH40H
A(*) B(t)
100.0 0.0
1,00.0 0.0
c(t)
0.0
0.0
D(t)
0.0
0.0
Curve
Linear -6
Li_near
-6
Timed events:
Initial states:
Switch L:No change
Switch 2:No change
Switch 3:No change
Swj-tch 4:No change
Time(min)
0. 00
EvenE
Switchl
Action
No change
Monday, February 12, 2007 12:55:05
Z'v VVc'
ri\
Parameter
page 2 of
fnstrument Method:
EDTA Pos Swabs.meth

LCQ Instrument Met.hod
Creator : Administrator
Last modified 2/9/ 07 by Administrator
MS Run
Time (min) : 10.00

MS
Detector Settinqs:
Segment 1 Information
Duration (min): 10.00

Number of Scan Events: 2
Tune Method: EDTA_Pos_CID
Scan Event Details:
l-:
Pos
MS/MS
2:
Pos
MS/MS
- (293.0)->o(tZS.0-315.0)
: CE 1-5. 0?
(0",
v,trn.,>) Ap
IsoW 1.0
. (305.0)->o(tZS.0-31_5.0)
: CE l-5. 0e IsoW 1. 0
20A7 L2246242
f-<. q(u
( ato\
Page I of
InsLrument Met.hod:
EDTA_Pos_Swabs
meth
Syringe draw rate (pl,/sec) :2.50
Tnicnf
inn
/"I\,q :5
"vrsne (pL)
rrnl"-o
settings:
Solvent A: 5: 95 ACN: l,f ater +
Solvent B: B
Pump
.
S6l \t6hf
0.
06*
NH4OH
a. n
Solvent D: D
Min pressure (pSI):0
Max pressure (pSI) :5000
Ch: ri
nrlf _.. -D--essure
^rrf
Chart output:Normal
Gradient program:
Time(min) Flow(mI,/min) A(t) B(E)

0.00
0.30
100.0 0.0
3. 00
0 . 30
100.0 0. 0
C(t)
0. 0
0. 0
D(E)
O. 0
O. O
Curve
Linear _
Linear _
Timed events:
Tn i f i a l
Switch
Switch
Switch
Switch
L:No change
2:No change
3:No change
4:No change
(min)
00
Event
Switchl
Tj.me
0.
qt- ri6a.
Act
j.on
parameter
No change
2OO7 12:46:42
&qq6
(
st,\
Page
2 of
METITOD
,/qb
1; r-t)
Instrument Method:
EDTA Neq Swabs.meth

LCQ
Instrument Method
Creator : Administrator
Last modified: 2/9/07 by Administrator
MS Run
Time (min) : 10.00

MS
Detector Sett.inqs:
I Information
Duration (min) : l-0.00
Segrnent
Tune Method:
EDTA_NEG
Scan Event Details:

l:
Neg - (291.2)->oS (246.5-247.5 272.5-273.5)
MS/MS: CE 15.0? Isow 1.0
2: Neg . (303.2)->oS(292.8-284.3)
MS/MS : CE l-5. O? IsoW 1. 0
3: Neg . (344.2)->oS (299.5-300.5 325.5-326.5)
MS/MS: CE 15.0? rsow 1.0
4:
Neg
- (356.0)->oS(31j-.5-312.5)
MS/MS: CE 15. O? IsoW L. 0
Friday, February
09, 2007 12:47:03
f-x (qa
(at z\
Dana
rgYU
1
+
n
v!
Instrument Method:
EDTA Necr Swabs.meth

lnjector parameters:
Syringe draw rate (F1lsec):2.50
fnjection vol-ume (p1) :5
Prrmn
c6f
l- i nfic
Solvent A:80:20 ACN:Water + 0.03t
NH4OH
SoLvent B:B
Solvent C:C
Solvent D:D
Min oressrrrc lPSf):0
Max pressure (PSI) :5000
Chart output: Pressure
Chart output:Normal
Gradient program:
Time(min) Flow(ml,/min) A(t)
B(t)
0.00
0.30
100.0 0.0
3.00
0.30
l-00.0 0.0
C(E)
0.0
0.0
D(t)
0.0
0.0
Curve
Linear Linear -
6
6
Timed events:
Tni ii r1
ei-rl-oc.
Switch
Swltch
Switch
Switch
(min)
0.00
Time
L:No
2:No
3:No
4:No
change
change
change
chanoe
Event
SwitchL
Action
No chanqe
Pararneter
Friday, February 09, 2007 1-2247 203
a4 lqb
/t> u\
page 2 of
SELECTIVITY
fu
44b
(^r t)
Seq uence---select_pos. sld [O pen]
t
Sample Name:
C-
A, Case 1, Grey
nent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample Type Ftle Name
Sample lD
Path
Unknown
C:\)(calibuAData\EDTA\BreweASEL
SELOl
Inst Method
Proc Method
CalFile

Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
Positive
Position
InjVol
5.0
Level
Sample Wt
0.000
*****************************i*****i**t********+********************************i*******t*t***tt**i***********t*********
Sample Name: Swab.A, Case 2, Red

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
02
C:Xcalibur\Data\EDTA\BreweASEL Positive
SELO2
Inst Method
Proc Method
Cal File

Vol
0.000
ISTD Amt
Dil Factor
0.000
t.00u
Position
InjVol
5.0
Level
lSample Wt
0.000
6u
/* q+b
1; t,')
page
zf t
lot
Seq uence--select_pos. sld [Open]

Sample Name: Swab B, Case 2, Grey
C'
-nent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
SELO3
03
C:U(calibur\DataEOtffi
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
*t**t**t**********ii*t***********t**t*****************************t*****ti****i***tr****t*******th*r
Sample Name: Swab C, Case 3-1, Grey

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
iample Type File Name
Sample lD
Path
lSEL04
04
C:Xcalibur\Data\EDTA\Brewer\SEt positive
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
Unknown
*******************t*************i**************tt*t*******t******t***********t****************t******************ffi***********************
6v
{"
(
q4e,
nt)
zf
rl.t
Sequence--select_pos. sld [Open]
Sample Name: Swab C, Case 3-2,
/--lment:
Study:
Client:
Laboratory:
Companyi
Phone:
Sample lD
Path
Unknown
SELOs
05
u : \Acail0u nData\E DTA\B reweAS EL_positive
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
******t*t***i*ti**********i*****t*********t**********************t******************************************H****************r********ttt*t***
Sample Name: Swab
'
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
***t**t*i***t*t*t********i**********************+*****************a*************************i*******t*************************************t***
4 rylu
(a )s)
ffi
zlnl't
Seq uence---select_pos. sld [Open]

Sample Name:
C'
b D, Case 3*4,
rent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Unknown
07
SELOT
Inst Method
C:XcalibuAData\EDTA\BreweASEL Positive
Proc Method
Cal File
C:XcalibuAmethods\EDTA Pos Swabs

Sample Vol
ISTD Amt
DilFactor
0.000
0.0rJ0
1.000
Position
InjVol
5.0
Level
Sample Wt
0.000
Sample Name:iSwab D, Case 4-1, Red

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
unKnown
08
C:U(calibur\Data\EDTA\Brewer\SEL Positive
SELOS
Inst Method
Proc Method
u:v(calrbur\metnods\tu
lA Pos swabs
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Cal File
Position
InjVol
5.0
{o qq,
(an)
Level
Sample Wt
0.000
6r
>lnln
Seq uence---select_pos. sld [Open]

Sample Name:
C-
, Case 5, Red
rent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
09
C:\XcalibuAData\EDTA\BreweASEL
SELOg
Inst Method
Proc Method
CalFile
C:\Xcalibur\methods\EDTA Pos Swabs

Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
Postlive
Position
InjVol
5.0
Level
Sample Wt
0.000
*t***********t**i**tt**********t**********************s******s***i********rl***********
Sample Name:
ellow
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
10
C:Xcalibur\Data\EDTA\Brewer\SEL Positive
SELlO
Inst Method
Proc Method
Cal File
u:u(cattbunmethods\EDTA Pos swabs

Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
Position
lnjVol
10
5.0
r( axc)
{v
a4
Level
Sample Wt
0.000
Ll,fu
Seq uence--select_pos. sld [Open]

Sample Name: Swab A, MAL, Yellow, d
C- 'nent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
11
C:U(calibur\Data\EDTA\Brewer\SEL
SELl
Inst Method
Proc Method
Cal File

Sample Vol
ISTD Amt
DilFactor
U.UOO
0.000
1.000
Positive
Position
lnjVol
11
5.0
Level
Sample Wt
0.000
*tl**********************t******t****t*********t**i**************************t**t********t***************
Sample Name: Swab D, MAL, Yellow, d12

Comrnent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Unknown
12
SEL12
lnst Method
ath
C:Xcalibur\Data\EDTA\Brewer\S
Proc Method

Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
CalFile
EL Positive
Position
12
qq u
t.(1u,1
njVol
5.0
Level
Sample Wt
0.000
{eul
tl't
.,,
i*,a,ru, 0...r.
l-eo,
181
00-l
go-.1
I
2.57
itiu(Gi]\
02109107 10:57:05
NL:4.76E3
rn/z='159.S160.5 .
F: + c ESI Full msz
1
r-
SwabA, Cdsdl.ErEV--.
/
____1
Selul*/5-96 RI: 0.96-1.27 AV: 12 NL:8.71E3

F: + c ESI Full
ms2 293.00@15.00 [ 125.00-315.00]
293.00@15.00 [
125.00.315.00t MS
Set0l
8.28E3
ntlz= 246.5-247.5
F: + c ESI Full ms2
293.00@1s.00 [
125.00-315.001 MS
SelOl
o
6
E
o
G
m/z= 167.t168.5
F: + c ESI Full ms2
30s.00@15.00 [
12s.00.315.001 Ms
Selo1
AV:9 NL: 1.16E4

: + c ESI Full ms2 305.00@15.00 [125.00-315.001
erurF64-1ul Kt:1.',Iu-1.3'l
6.46E3
rn/z= 258.$259.5
F: a c ESI Full ms2
305.00@1s.00 [
125.00-31s.001 Ms
Sel0'l
o
o
c
o
o
-s!
NL:6.89E4
TIC MS Sel01
L,t 4
(a
NL:4.76E3
m/z= 159.5-160.5
F: + c ESI Full ms2
293.00@15.00 [
125.00-315.001 MS
Sel01
mlz= 246.5-247.5
F:+ c ESlFull ms2
293.00@15.00 [
197
2.58
12100-315.001 MS
277
3.63
miz= 167.5-168.5
F: + c ESI Full ms2
30s.00@1s.00 [
125.00-315.001 MS
Sel01
q.,
.z
o
E
x.
mlz= 258.5-259.5
F:+ c ESI Full ms2

305.00@1s.00 [
125.00-315.001 MS
Sel01
TIC MS
Sel01
f.'L+u
Tima /minl
(av
t\
0?/09107 10:57:05
el01#E4-87 RT: 1.11-1.14 AV:
NL:1.37E3
m/z= 159.$160.5
F: + c E5; 5u1
293.00@1s.00 I
atr(
NL: 6.7SE3-
+ c ESI Full ms2 293.00@1S.00

[ 125.00-315.00]
.",
125.00-315.001 MS
Sel01
o
G
E
o
o
@
rnlz= 167.5.168.5
F: + c ESI Full msz
30s.00@15.00 [
125.00-3'15.001 MS
Sel01
o
o
6
u
o
=
.g
6.03E4
TIC MS Sel01
+ c ESI Full msz 305.00@15.00
NL: 2.93E4
125.00-31s.001
\-1
:U(qalibur\...\Sel-PositivEffi)
n_
0U09107 10:57:05
NL: 1.37E3
rniz= 159.S160.5
F: + c ESI Full ms2
2e3.00@15.00 I
125.00-315.001 MS
A, Case 1, Grey
Sel01#90-95 RT: 1.19-1.24 AV:3 NL: 1.16E4

F: + c ESI Full ms2 293.00@15.00 [ 125.00-315.001
Selol
6.1 9E3
.ll'lz= 246.5-247 ,5
F: + c ESI Full ms2
293.00@15.00 [
125.00.315.001 MS
o
o
6
!
!a
o
o
o
n/z:167.5-16E.5
F: + c ESI Full msz
305.00@1s.00 [
'125.00-3't5.001 Ms
Sel0'l
+ c ESt Fult ms2 305.00@15.00
:9.ZJEJ
rn/z= 258.5-259.5
F: + c ESI Full ms2
305.00@15.00 I
r25.00-315.001 Ms
Selo1
o
o
6
E
0
6
NL:6.03E4
TIC MS Selol
6,t
(as
12s.00-315.001
aap
02109107 11:08:17
NL:0
Swab A, Case 2, Red
: + c ESt Fuil ms2 293.00@15.00 [ 125.00-315.001
rvz= I 59.5.1 60.5

F:+q551 5u11.O
293.00@15.00 [
125.00-315.00r MS
Selo2
rlz=
o
o
o
246.5-247.5
F: + c E51
Pu11
*,
2e3.00@15.00 [
12100-315.00] MS
o
6
+ c ESI Full ms2 305.00@15.00 12S.OO-glS.OO]

[
NL:7.66E3
rn/z= 258.5-259.5
F: + c ESI Full ms2
30s.00@15.00 [
125O0-315.001 Ms
o
6
.=
ro0l
170
z.1J
2'?6 nz
NL:6.62E4
"g!
TIC MS Sel02
,o-]
*.1
158
184
1
ro-l
uo-l
200
6,/ tb
r.-/5
C:Vcalibur\...rSel-eositiv@lD
02109107
11
:19:06
Swab B, Case 2, Grey
tuJrcz-tu Kt: u.6z{r.9u AV: 4 NL: 0
NL:0
rvz= 159.5.160.5
+ c ESI Full msz 293.00@'t5.00 125.00-315.001

[
F: +c95; 6u1,r.,
293.00@15.00 [
125.00-315.001 MS
Sel03
rnlz= 246.5-247 .5
o
o
293.00@1s.001
125.00-315.001 MS
Sel03
F:+cESl Fullms2
':
.s!
trVz= 157.5.168.5
F: + c ESI Full ms2
305.00@15.00 [
12100-315.001 Ms
uJ#62-6C Kt: l.Uir-].10 AV:
NL: 2.ggE3
+ c ESI Full ms2 305.00@1S.00

[ 12S.OO-315.00]
2.51E3
r/z= 258.$259.5
F: + c ESI Full ms2
?33.339i;trt*
o
o
E
.=
2.99E4
TIC MS Sel03
{.v
LqJ
-l0E
C :U(na I ibu
r\...\SEL-Positiv(@
0U09107 11:29:58
_--'
Swab C, Case 3-1, Grey)

(--__-_____-_-j-
tu4*ttz-tu Rt:0.62.0.90 AV:4 NL:0
NL:0
+ c ESI Fuil ms2 293.00@15.00 125.00-315.001

[
rn/z='159.5.160.5
F: + c ESI Full ms2
i!"3#.9t33&r*
tnlz= 246.5-247 .5
F: + c ESI Full ms2
293.00@15.0o I
125.00-315.001 Ms
o
o
uo
o!
o
.s!
r/z='167.5.168.5
F: + c ESI Full ms2
305.00@15.00 [
Ms
33r5d!0-31s.001
I
+ c ESI Full ms2
r/z= 25E.5-259.5
F: + c ESI Full ms2
305.00@15.00 [
125.00-3't5.00t Ms
SetM
o
o
o
E
4
o
,z
{nu
(as
15.00 [125.0G315.00]
z--T':^
0?J09rc7 11:40:49
NL:O
lF; + c
rvz= 159.5-'160.5
)uv
rU
I:
U.62.{J.9U AV: 4 NL: O

Full ms2 293.00@1s.00 [ 125.00-31S.00]
X
F: + c ESI Full ms2
ffi81319'ir"'
o
o
oo
o
.=
o
o
nr/z= 167.$'168.5
F: + s E51 Prt
r.,
i:fig3eJifir".
;;dii;ljri'!2-ift
mts= 258.$259.5
F: + c ESI Full ms2
305.00@1s.00 [
12100.315.001 MS
o
6
3E5
MS Sel05
1.1
&,
(at
:d;6"is.,jt'r12s.00-3is.oot
C:\Xcalibur\...\SEL Positiv
I
0?J09107 11:51:40
----<--)
'u xt;
NL: O
m/z= 159.5-160.5
F: + c ESI Full ms2
293.00@1s.00 t
12s.00-315.001 Ms
Sel06
u.bz{J.gu
Av:4
NL:0
Full ms2 293.00@1s.00 [ i25.00-31S.00]
o
E
o
J
o
6
o
rn/z= 167.5,'168.5
F: + c ESI Fult ms2
305.00@1s.00 t.
t s. ool' r,ls
32",5d30-3
efub*rur-r/6 Rr: 2.11-2.31 AV: 16 NLi 6ZSE

: + c ESI Full ms2 305.00@is.oO 1 rzS.oo:eiS.oOl
m/z= 256.$259.5
F: + s E51 Prt
rs2
U3;l3e;3f3rr^
o
o
o
o
o
NL: 1.37E5
TIC MS Sel06
)t)
C:U(calibur\...\SEL
0U09lO7 12:02:31
utnz-tv
Swab D, Case 3-4,

r t; u.6z-u,9u AV: 4
NL: 0
+ c ESt Fuil ms2 293.00@15.00 125.00-315.00I
[
NL:0
rn/z= 159.5-160.5
F: + c ESI Full ms2
293.00@15.00 [
12s.00-315.001 Ms
Sel07
I
G
o
l9
o
fil/z= 167.t168.5
F: + c ESI Full ms2

305,00@15.00 [
12530-315.001 Ms
T: + c ESI Full ms2 3o5.oo@1s.oo t 125.06iJ
rn/z= 258.S259.5
F: + c ESI Full ms2
?3*339t33&r",
uo
o
'NL: 1.25E5
TIC MS Sel07
fo'/
( aq,
.s!
-YrF
C:U(calibun...\SEL
t-
positive{ffi;)
OZ09l07 12:.13:2'l
NL: 0
+ c ESI Full ms2 293.00@15.00 125.00-315.00]

[
n/z= 159.$160.5
F: + c ESI Full ms2
293.00@15.00 [
125.00-3't5.001 MS
Sel08
c)
o
E
o
.a
.g
ruz= 167.$168.5
F: + c ESI Full ms2
30s.00@1s.00 [
12100-315.001 Ms
m/z= 258.$259.5
F: + c ESI Full ms2
305.00@1s.00 [
'125.00-315.001 MS
736 Sel08
9.68
o
o
o
.:o
s
NL:'1,15E5
TIC MS Sel06
6,
c ESI Full ms2 305.00@15.00 [ 125.00-3tS.O0l
an
NL:0
rn/z= 159.5-160.5
F: + c ESI Full ms2
+ c ESt Fuil ms2 293.00@15.00

[125.00-315.001
.Yr.uu(4 to.uu t
125.00-315.001 MS
Sel09
8.85
I
n:/z= 246.5-247 .s
F: + c ESI Full ms2
293.00@15.00 |
125.00-31
5.001'Ms
Full ms2 305.00@15.00 [ 125.00-31S.00]
ntz= 25E.5-259.5
F: + c ESI Futt ms2
305.00@15.00 t
12100-315.001 Ms
TIC MS Sel09
02t09t07 12..35..M
Swab A, MAL. Yellow
+ c ESI Fuil msz 293.00@.t5.00 125.00-315.001

[
trVz= 159.$160.5
F: + c 551 Pr;;
293.00@1s.00 I
125.00-315.001 MS
t",
: E. l4E3
fil/z= 246.5-247.5
F: + c ESI Full ms2
?i3:33913331t*
0
o
6
.:o
6
9.97E2
nvz= 'l 67.5-1 68.5
1001
F: + c ESI Full ms2
j!fli&ets,lerr*
'o-]
'o-l
,n_j
m82 305.00@15.00 [ 125.00-315.001
100-l
9a
rso
go-l
*-l
,^l
'"t
168
144
182
uo-]
't8/.
1
t"
(
qq
aq+
rXcalibuA...\SEL-eo.itiu@
0?/09107 12:45:5,4
Swab A, MAL, Yeltow, OiZ
: + c ESI Fuil ms2 293.00@15.00 [ 125.00-315.00]
nvz= 159.$160.5
F: + c ESI Full ms2
293.00@15.00 [
125.00-315.001 MS
rtlz=246.5,247.5
F: + c ESI Full ms2
293.00@15.00 [
125.00-315.001 MS
Salt'l
o
o
o
[ 125.00-315.001
.a
ddtrt
rn/z= 258.$259.5
F: + c ESI Full ms2
305.00@15.00 [
125.00.315.001 MS
Sel1l
I
u6
o
6
i.94
150
NL:
Ilc
MS
Selll
fr'l(
(v
spifea-\
{bF
"TI'F
02109107 12:57:01
NL:0
+ c ESI Full ms2 293.00@15.00 [
rn/z= 159.$160.5
F: + c ESI Full ms2
293.00@1s.00 [
'125.00-315.00t MS
Sel12
'Itlz= 246.5-247.5
F: + c ESI Full ms2
293.00@1s.00 [
125.00-315.001 MS
Sel12
!)
6
f
!
o
o
et14t4-tI Kr: U.97-l.OO AV: 2
NL: 1.22E4
: + c ESt Full ms2 305.00@15.00 [125.0015.00]
dz= 258.$259.5
F:+cESl Fullms2
30s.00@1s.00 [
125.00-315.001 MS
Sel
l2
o
o
E
o
100-]
;l--l
-l
za)
uo-]
3.0'1E5
MS Sel12
.z
6
o
Seq uence--select-neg. sld [Open]

Sample Name: Swab A, Case
1,
'"nent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
Sel01
Proc Method
lnst Method
C:U(ca
I i
bu
:Xcalibur\Data\EDTA\Brewer\S
Cal File
r\methods\EDTA-Neg-Swabs
Sample Vol
0.000
STD Amt
L_Negative
Position
InjVol
5.0
Sample Wt
Level
0.000
DilFactor
1.000
0.000
, Case 2, Red
Sample Name:
Study:
Comment:
Glient:
Laboratory:
Company:
Phone:

Unknown
Sel02
Samole lD
Path
02
Xcal
bu
Proc Method
lnst Method
C
AData\EDTA\Brewer\S
Cal File
U(ca li bu r\method s\EDTA_Neg_Swabs
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
L_Negative
Position
InjVol
5.0
,Level
Sample Wt
0.000
*****tt***********t***********************#**********t***r**********
,49
;r*u'
C"+4a
( att)
paqe
Seq uence---select_neg. sld [O pen]

Sample Name: Swab B, Gase 2,
rent:
Study:
Glient:
Laboratory:
Company:
Phone:

Sel03
Unknown
Sample lD
Path
03
C:Xcal
Proc Method
lnst Method
C
Xcalib
ibu
r\Data\E DTA\BreweASEL_N egative
Cal File
Amethods\EDTA_Neg-Swabs
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Position
lnjVol
5.0
Samole Wt
Level
0.000
Sample ttame:
Comment
Study:
Client:
Laboratory:
Company:
Phone:
Type File Name

Sel04
Unknown
Sample lD
Path
04
Proc Method
nst Method
C :U(ca
li
bu
:U(calibu r\Data\EDTA\Brewer\S
r\methods\EDTA-N eg-Swabs
Sample Vol
ISTD AMt
Dil Factor
0.000
0.000
1.000
CalFile
L_N egative
Position
InjVol
5.0
Level
rSample Wt
0.000
4rtt*t"
, ++,lrq s)
Seq uence--select_neg. sld [Open]

Sample Name:
.ment:
Study:
Client:
Laboratory:
Company
Phone:
Sample lD
Path
Unknown
05
C:Xcalibur\Data\EDTA\Brewer\SEL Neqative
Sel05
Inst Method
Proc Method
Cal File
G:Xcalibur\methods\EDTA Neo Swabs

Sample Vol
ISTD Amt
Dil Factor
0.000
U.OUO
1.000
Position
InjVol
5.0
Level
Samole Wt
0.000
Sample Name: Swab C,

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
unKnown
06
Sel06
Inst Method
:Xcal
ibu
Proc Method
AData\EDTA\BreweAS EL_Negative
Cal File
A_Neg_
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Position
InjVol
5.0
44u
aq ri\
Level
]Sample Wt
0.000
oJf'
Sequence--select-neg. sld [Open]

Sample Name:,Swab D, Case 3-4, GreY
('
rent:
Study:
Client:
Laboratory:
Company:
Phone:

Sel07
Unknown
Sample lD
Path
07
Proc Method
lnst Method
C : U(cal ibu
:Xcal ibu r\Data\E DTA\Brewer\SE L-Negativg
CalFile
r\meth ods\E DTA-Neg-Swabs
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Position
lnjVol
5.0
Level
Samole Wt
0.000
Sample Name: Swab D, Case 4-1,

Study:
Comrnent:
Client:
Laboratory:
Company:
Phone:
Sample Type File
Name
Sel08
Unknown
lSample lD
08
li
bu
:\)(cal ibu r\Data\EDTA\B rewer\SEL-Negative
Proc Method
lnst Method
C :U(ca
Path
r\method s\EDTA-Neg-Swabs
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
CalFile
Position
InjVol
5.0
ty- 4ab
('u4
Level
Sample Wt
0.000
/s"9
r\' M
Seq uence--select-neg. sld [Open]
,-|'
D, Case 5,
Sample Name:
Study:
nent:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
09
Sel09
Proc Method
lnst Method
C
:Xcalibun\Data\EDTA\Brewer\SEL-Negative
CalFile
:U(cal i bur\methods\EDTA_Neg_Swabs
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
Position
InjVol
5.0
Level
Sample Wt
0.000
Sample Name:lSwab A, MAL, Yellow

Study:
Comment:
Client:
Laboratory:
Gompany:
Phone:

Unknown
Sel10
Sample lD
Path
10
U(calibu r\Data\E DTA\Brewer\S
Proc Method
lnst Method
C
:U(cal i bu r\methods\EDTA-Neg-Swabs
Sample Vol
ISTD AMt
DilFactor
0.000
0.000
1.000
Cal File
L-N eg ative
Position
InjVol
10
b.0
L,{/^ L{+(( Joi)\
Level
Sample Wt
*Jt*,"
Seq uence--select_neg. sld [Open]

A, MAL, Yellow, d12
Sample Name:
t'
'ment:
Study:
Client:
Laboratory:
Cornpany:
Phone:
Sample lD
Path
Unknown
11
Sel11
Inst Method
C
:Xcal
ibu
:U(cal ibur\Data\EDTA\BreweAS
Sample Vol
ISTD Amt
Dil Factor
U.UUU
0.000
1.000
L_Negative
Position
lnjVol
11
5.0
Sample Wt
Level
0.000
, MAL, Yellow, d12 spiked
Sample Name:
Study:
Comment:
Client:
Laboratory:
Company:
Phone:

Sel12
Unknown
Sample lD
Path
12
Proc Method
lnst Method
C U(cal ibu
:
:V(calibur\Data\E DTA\B reweAS EL_Negative
r\meth od s\EDTA_N eg_Swabs
Cal File
Position
InjVol
12
5.0
Sample Wt
Level
r0.000
I
Samole Vol
ISTD Amt
Dil Factor
O.UUU
0.000
1.000
to +*a
( sa),
ualzlvl
1uiz1:J4
DWaO
A, \JaSC |, lJrt,y
NL:2.96E4
rnlz=272.5-273.5 F: - c
ESI SRM ms2
291.20@15.00 I
?46.50-247.50,
272.50-273.501 MS
Sel0l
1001
NL: 1.08E4
rniz= 299.5-300.5 F:
ESI SRM ms2
344.20@15.00 I
299.50-300.50.
325.50-326.50t MS
Sel01
m'lz= 246.5-247 .5 F: - c
ESI SRM ms2
ESI SRM ms2
291.20@15.00 [
246.50-247.50,
272.50-273.s01 MS
;il
ssl
J'r
34420@15.00 [
299.50.300.50.
325s0-326.501 MS
Sel01
80-l
"-]
ro-l
.u-l
8
60-.'l
nJz= 282.V2U.3F: - c
ESI SRM ms2
ESI SRM msZ

356.00@15.00 [
303.20@1s.00 [
282.7U2U.251 MS
31r5G312.501 MS
Sel01
tp
Time (mn)
aU
( sat
Time (min)
-c
02112107 10:32:28
Swab A, Case 2, Red
nr/z= 299.S300.5 F: - c
ESI SRM ms2
344.20@15.00 I
,oo qn_1nn 6n
32s.50.326.501 MS
Sel02
3.91 E4
nvz= 325.S326.5 F: - c
ESI SRM msz
344.20@1s.00 I
299.50-300.50,
325.50-326.501 MS
Sel02
nlz=246.*247.5F.-c
ESI SRM ms2
29r.20@1s.00 [
246.50-247.50.
272.s&273.501 MS
Sel02
1.29E3
m/z= 31'1.5-312.5 F:- c
ESI SRM ms2
3s6.oo@15.00 [
311.50.312.501 MS
Sel02
filz= 282.8-2U.3F:. - c
ESI SRM ms2
303,20@15.00 I
282.7t284.2s1 MS
Sel02
[,
Time (min)
v+
(t,o)
Time (mrn)
C:U(calibuA...\SEL-Neeafiv@!],/
02112J07 1O:43:17
Swab B, Case 2, Grey
NL:1.92E4
00-l
ilz=272.5-273.5F: - c
ESI SRM ms2
29120@15.001
^^l
246.50-247.50.
272,50-273.501 MS
Sel03
"r-l
Ir'lz=246.5-247.5Fi - c
ESI SRM ms2
291
20@15.00 [
246.9-247.fi.
272.50-273.501 MS
Sel03
o
.E
10(
nlz=282.8-28/..3F:. - c
ESI SRM ms2
9:
303:0@1s.00 [
282.7$.284.2s1 MS
8:
80
7t
70
4
55
40
30
Time (min)
Tlme (min)
JAP
C : u{ca
bu
021207 10:54:09
4...\S e L-N e gaIv(\Se to1)
,Jr/13
Swab C, Case 3-1, Grey
NL: 1.21 E4
trl/z= 299.5-300.5 F: - c
ESI SRM ms2
344.20@15.00 I
299.50-300.50,
325.50-326.501 MS
Sel04
NL: 1.34E4
ttlz= 272.5-273.5 F: - c
ESI SRM ms2
291.20@15.00 [
246.50-247.50,
272.5&273.501 MS
Sel04
rn/z= 325.$326.5 F: - c
ESI SRM msz
344.20@15.00 [
299.50-300.50,
325.50-326.501 MS
Sel04
o
d
o
o
NL: 3.74E3
mlz=282.8-2U.3 Fi - c
NL: 7.73E3
r/z= 31 1.5-312.5 F: - c
ESI SRM ms2
282.7s.2U.251 MS
356.00@15.00 [
311.50-312.501 MS
Sel04
Sel04
ESI SRM m2
303.20@15.00 [
tr- u,l
Time (min)
&4
ilx
Time (min)
0212107
C:XcalibuA...\SEL_Negativ{9eP
't
1:04:58
Swab C, Case 3-2, Red
NL: 5.04E3
m/z= 299.$300,5 F: ESI SRM msZ
3,14.20@15.00 I
299.50-300.50,
325.50-326.501 MS
Sel05
NL: 1.09E4
272.$273.5 F: - c
ESI SRM ms2
291.20@15.00 [
246.50-247.50,
272.50-273.501 MS
Sel05
ftUz=
10(
tt!z= 246.5-247 .5 F: - c
ESI SRM msz
29120@15.00 [
9l
AI
r/z:325.5-326.5 F: - c
ESI SRM ms2
3,14.20@15.00 [
299.50-300.50,
325.50-326.501 MS
Sel05
246.50-247.50,
272.50-273.501 MS
Selos
9(
J I'P
8(
7l
7(
8et
Ss.
E
6
10c
.r/z= 282.8-28/'.3 F: - c
ESI SRM ms2
303.20@15.00 [
282.75-284.251 MS
Yi
r/z=
31 1.5-312.5 F: - c
ESI SRM ms2
356,00@15.00 [
311.50-312.501 MS
DEIUJ
8t
Af
7,
7C
CL
45
40
30
f"
qs
( s'"t)
Time (min)
Time (min)
:Xca
ib q
4...\S e
l-ru"S"tiu{@
02/12/0711:15:48
Swab C, Case 3-3, Grey
NL;4.26E4
nlz= 272.5-273.5 F: - c
NL:1.20E4
m/z= 299.5-300.5 F: - c
ESI SRM ms2
344.20@15.00 I
299.50.300.50,
325.50.326.501 MS
Sel06
ESI SRM ms2
291.20@15.00 [
246.50-247.50,
272.50-273.501 MS
Sel06
1.88E4
rnlz= 246.t247.5 F: - c
ESI SRM ms2
291
z,otE5
rtz=
.20@15.00 [
o
.E
nlz= 282.8-28/.3 Fi - c
ESI SRM ms2
303.20@15.00 [
282.75-2A4.251 MS
Sel06
90
80
70
65
60
55
45
40
t<
30
Time (min)
msz
344.20@15
344.20@15.00
[
299.50-300.50,
299.50-300.
32s.50-326.501 MS
93
325.5-326.5 F: - c
ESI SRM
246.fi-247.50.
2725o-273.50i Ms
100
:TOP
Time (min)
02112107 11:26:37
C:Xcalibur\...tSEt-t tegativdsepZ)
Swab D, Case 34, Grey
NL:7.88E3
NL:4.74E3
1
00-t
$lz=272.$273.5Fi
*1
ESI SRM ms2

291.20@15.00 [
aq!
*t
10r
m/z= 299.5-300.5 F: - c
ESI SRM ms2
u420@15.0O1
299.50-300.50,
325.50-326.501 MS
246.50-247.il,
272.s0-273.501 Ms
Selo7
Sel07
'-l-.
70-J
oci
*.]
sq
i2.23Eg
1.96E4
trVz= 325.5-326.5 F: - c
ESI SRM ms2
nn-246.*247.5Fi -c
ESI SRM ms2
344.20@15.00 [
299.50-300.50,
32s.50-326.501 Ms
29120@1s,00 I
246.fi-247.50.
272.s0-273.50i MS
Sel07
Sel07
o
c
6
b.ZYEJ
ntlz= 311.5-312.5 F: - c
ESI SRM ms2
3s6.00@15.00 I
31 1 .50-312.501 MS
'r'lz=282.8-2U.3F: - c
ESI SRM msz
30320@15.00 [
282.75-284.251 MS
Sel07
S107
[y +,/a
( tor)
Tlme (min)
Time (min)
02i1U07 11:37''28
C:D(calibuA...\SEL_NeOativQp)
Swab D, Case 4-1, Red
NL: 1.85E4
rn/z= 299.5-300.5 F: - c
ESI SRM ms2
344.20@15.00 [
299.50-300.50,
325.50-326.501 MS
Sel08
NL: '1.48E4
mlz= 272.5-?73.5 F: - c
ESI SRM ms2
291.20@15.00 [
246.50.247.50.
272.50-273.501 MS
Sel08
100
90
rol
nlF
1.O7E4
m/z= 325.$326.5 F: - c
ESI SRM ms2
344.20@15.00 [
299.50-300.50,
325.50-326.501 MS
246.*247.5 Fi - c
ESI SRM ms2
ru-l
29120@15.00 [
246.50-247.50,
272.50-273.s01 MS
Sel08
ro-i
,l
-rbp
SelOS
E0-l
75-]
I
::.1
"l
60-]
ol
3
NL:7.79E3
nlz=282.E-2U.3 F: - c
30320@15.00 [
282.75-284251 MS
rn/z= 311.F.312.5 F: - c
ESI SRM ms2
356.00@15.00 [
311.50-312.501 MS
Sel08
SelOS
ESI SRM ms2
'nme (min)
'nme (min)
, C:U(balibuA.,.rSel-rueOativ@
lool oft
'll
s'l
02112107
1 1
:48:16
Swab D, Case 5, Red
wp
mlz= 272.1273.5 F: - c
ESI SRM ms2
291.20@15.00 [
246.50-247.50,
272.50-273.s01 MS
Sel09
ff{z= 246.5-247 .5 F: - c
rn/z= 325.5-326.5 F: - c
ESI SRM ms2
344.20@15.00 I
299.50-300.50,
325.50-326.501 MS
Sel09
ESI SRM ms2
29120@1s.00 [
246.fi-247.50.
272.s0-273.501 MS
Sel09
o
d
E
e
@
Io
E
rtlz= 282.8-2U.3
F'.
-c
ESI SRM ms2

303.20@15.001
282.75-284.251 MS
Sel09
ESI SRM ms2

3s6.00@1s.00 [
311.50-312.501 MS
Sel09
[* uu,
( s")
Time (min)
Time (min)
02112107 11:59:08
, C:U(calibuA...\SEL-NeSativgi
Swab A. MAL, Yellow
-J
Dtt'
NL: 9.55E3
1
00t
rn/z:299.$300.5 F: - c
*l
ESI SRM ms2

344.20@15.00 [
299,50-300.50,
325.50-326.501 MS
*l
oni
Sel10
1001
z.vlEJ
rl/z= 325.$326.5 F: - c
lAEA
rlz=
246.5-247 .5 F'. - c
ESI SRM ms2
ESI SRM ms2
34420@1s.00 [
299.50-300.50,
325.50-326.501 MS
2e1.20@r5.00 [
;;
246.50-247.fi,
272.50-273.s01 MS
Sel
,u-l
Sel10
l0
ro-.1
tul
att
'o-l
.o-]
ol
qvb
(2,)
Time (min)
Time (min)
:lXcalibu A...\S
EL-NeOati{}p
0?112107 12:10:01
Swab A, MAL, Yellow, d12 spiked
NL:2.06E3
dz= 299.5-300.5 F: - c
ESI SRM ms2
344.20@15.00 I
299.50-300.50,
325.50-326.501 MS
Sell 1
NL: 7.28E3
1001
nrlz=272.*273.5F: - c
ESI SRM ms2
291.20@1s.00 [
--l
,"1
246.50-247.50,
qnJ
--l
272.50-273.501 MS
Sell'l
rnlz= 325.5-326.5 F: - c
ESI SRM ms2
nlz=246.U24?.5F: - c
ESI SRM ms2
291 .20@15.00
246.fi-247.fi,
-JbP
344.20@1s.0o I
299.50-300.50,
325.50-326.501 MS
Sell l
272.50-273.s01 MS
Selll
o
o
o
:3.74E4
:1.'llE6
miz= 3'l 1 .5-312.5 F: - c

ESI SRM ms2
356.00@15.0o I
311.50-312.5O1 MS
ntlz=282.6-28/..3F:- c
ESI SRM ms2
303.20@15.00 [
282.7r2U.251
Sell'l
MS
Sel11
80
7
70
{n,tq{"
(t,t
Time (min)
Time (min)
0211A07 12'.20:51
lXcalibur\...\SEL-NeSativeEP
Swab D, MAL, Yellow, 01z sptKeo
NL:3.25E3
NL: 5.96E3
rool
nr/z= 299.$300.5 F: - c
ESI SRM msz
344.20@15.00 [
299.50-300.50,
325.50-326.501 MS
Sel12
r:.lz=272.5-273.5 F: - c
ESI SRM msZ
291.20@1s.00 (
nl
*l
246.50-247.fi,
272.sG273.s01 MS
Sel12
3.78E3
NLi 8.03E3
trtlz= 246.*247.5F: - c
ESI SRM ms2
291.20@15.00 [
1001
*-l
246.fi-247.&,
o.-l
Selt2
r/z= 325.$326.5
F: - c
ESI SRM ms2
r5.00 I
344.20@15.00
299.50-300.50.
299.50-300.50,
325.50-326.s01 Ms
Sell 2
272.s0-273.501 MS
*l
Jv7
80-l
'u-l
rol
*l
8 60-l
g -.
F
I
.E
1.03E4
r/z=
mlF 282.8-2u.3F'. - c
ESI
31
1.$312.5 F: - c
ESI SRM ms2

3s6.00@15.00 [
311.50-312.501 MS
Sel12
sRM ms2
303.20@15.00 [
282.7$284251 MS
Sell2
Time (min)
L.O.D.
{* qlb
(:is)
Sequence---LoD_neg. sld [Open]

Sample Name: 100 ppm EDTA
nent:
Study:
Client:
Laboratory:
Company:
Phone:

Unknown
LODOl
Proc Method
CalFile
Sample lD
Path
Inst Method
C:XcalibuAData\EDTA\Brewer\LOD NeoatMe g: V\calibur\methods\EDTA Nec

Position
lnjVol
5.0
,evel
Sample Wt
Sample Vol
ISTD Amt
u.000
0.000
0.000
r*****************

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Proc Method
Cal
File
Position
InjVol
5.0
Level
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
*********t**************t*************************************
fl+uu
(
stu)
nano
ft>[r'\o1
Sequence---LOD_neg.sld [Open]
nent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Unknown
LODO3
01
Proc Method
CalFile
Position
Path
:
Inst Method
U(calibu r\Data\EDTA\BreweALO D_Negative G:U(calibuAmethods\EDTA
njVol
Level
5.0
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
Nei
*******i*+*t*********t**t************tt**r********
Sample Name:
ppm EDTA
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample Type l-rle Name
Sample lD
Path
Unknown
02
Position
InjVol
5.0
LOD04
:U(calibu
lnst Method
r\Data\EDTA\Brewer\tO[Negative
Level
Xca
ibu r\m etn oO
s\EDTA_N e g
Sample Wt
Sample Vol
ISTD Amt
0.000
0.0u0
0.000
l********************************************i**********
5u a'/ b
G,r)
-yit
-vlvlo1
Sequence---LoD_neg. sld [Open]

nent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
LODO5
02
C:
Proc Method
CalFile
Position
lnjVol
5.0
Sample Name:
Inst Method
U(calibu r\Data\EDTA\Brewer\LOD_Negative
Level
G:
V(cal i bu r\method s\EDTA_Neg
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
ppm EDTA
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample Type
ile Name
Sample lD
Path
Unknown
LODO6
02
Proc Method
CalFile
Position
lnjVol
5.0
Xcali
Inst Method
bu
r\Data\E DTA\Brewer\LO D_Negative C:Xcalibur\methods\EDTA Nec
Level
Sample Wt
Sample Vol
u.uuO
0.000
ISTD Amt
**#*****************t*******************t************t********t
5,
I0Y
-O
4,/ e
3,s)
"tlpl"1
"t.
"
''
Sequence---LOD_neg. sld [Open]
rent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
LODOT
03
Proc Method
Cal File
Position
lnjVol
5.0
Inst Method
U(calibur\Data\EDTA\Brewer\LO D_N egative
Level
:v\caltbur\rnethods\EDTA Nec
Sample Wt
Sample Vol
ISTD Amt
u.000
0.000
0.000
f******i*******t*****i*************t********s******tr*t***************r*****************
Sample Name:
Study:
Client:
Laboratory:
Company:
Phone:
uample lype File Name
Sample lD
Path
Unknown
LoD08
]03
Proc Method
Cal File
Position
lnjVol
5.U
Inst Method
U(cali bu r\Data\EDTA\BreweALO D_N egative C:Xcalibur\methods\EDTA Neo
Level
- qq/o
(:^'^,\
Sample Wt
Sample Vol
ISTD Amt
0.000
rJ.u00
0.
7rV
vl,'lc1
'",'
Seq uence---LO D_neg.
sld [Open]
rent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
LODOg
03
Proc Method
CalFile
Position
InjVol
5.0
Inst Method
:Xcalibu AData\EDTA\B reweALOD_t',I
Level
eg
ative C:U(calibuAmethods\E DTA Nec
Sample Wt
Sample Vol
ISTD Amt.
0.000
0.000
0.000
******t*********
Sample Name:
ppm EDTA
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample Type
Unknown
ile Name
LOD1O
Proc Method CalFile
Sample lD
Path
04
C:U(calibu r\Data\E DTA\B reweAIOD_N egEtive U:\Xcatrbur\methods\EDTA Nec
Position
InjVol
Inst Method
Level
AA
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
****************t************r**s**************************s*****t****t*****
Quuu
ba)
ApU
Ylvl"1
Sequence--LOD_neg. sld [Open]
,
rent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
LOD11
04
Proc Method
CalFile
Position
lnst Method
:U(calibuAData\EDTA\Brewer\LO
njVol
Level
D_Negative C:\)(calibur\methods\EDTA Neo
lSample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
5.0
********t*********************t**t**********t******s***t****************t********************t****iis***********t**********ffi********
Sample Name: 13 ppm

Study:
Comment:
Client:
Laboratory:
Company:
Phone:
Samole lD
Path
lnst Method
:U(calibu AData\EDTA\BreweALO D-Negative C:U(calibur\methods\EDTA N
Unknown
LOD12
04
Proc Method
CalFile
Position
lnjVol
5.0
evel
Sample Wt
Samole Vol
ISTD Amt
0.000
0.000
0.000
****t***********
q,/,-
{o
( zt,\
zfo
JDY
)lru'\21
Seq uence---LOD_neg. sld [Open]

lent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Unknown
LOD13
05
Proc Method
Cal File
Position
lnjVol
5.0
Path
lnst Method
\/\Ldiluut \ua[a \tru I A\E'rewer\Luu_Nggatlv
Level
********t*tf
Sample Name:
:v(calibur\methods\EDTA
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
******************************t********i*****f
Nec
*r
ppm EDTA
Comment:
Study:
Client
Laboratory:
Company:
Phone:
Sample lD
Path
Inst Method
Unknown
LOD14
05
u : \xcatrbu r\Data\EDTA\B reweALOD_Negative
C:Xcalibur\methods\EDTA I'teo
Proc Method
CalFile
Position
InjVol
Level
lSample Wt
Sample Vol
ISTD Amt
0.000
0.000
5.0
0.000
.***************l***************tt********s**i
6. uoo
(sta)
Tr?
-t'ltvlal
.'",.,
Sequence---LOD_neg. sld [Open]

Sample Name:
ppm EDTA
Ytent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Unknown
LOD15
05
Proc Method
Cal File
Position
lnjVol
5.0
Path
Inst Method
:U(calibuAData\E DTA\B rewer\LO D-Negative u:v(calibur\rnethods\EDTA Nec

Level
Q vva
( t:z)
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
anT
'Vl'v\o1
0U1?i07 12:41:10
:\)(calibur\...\LOD-NeOativ@$
100 ppm EDTA
J"?
NL: 1.94E4
BVz= 299.5-300.5 F: - c
ESI SRM ms2
n/z= 272.5-273.5 F: - c
ESI SRM ms2
291.20@15.00 [
246.50-247.50,
272.50-273.501 MS
Lod01
34420@15.00 [
299.50-300.50,
325.50-326.501 MS
Lodo1
fl/z= 325.5-326.5 F: - c
fitlz= 246.+247.5 Fi - c
ESI SRM ms2

344.20@1s.00 [
299.50-300.50,
325.50-326.501 MS
ESI SRM ms2

291.20@15.00 [
246.50.247.50,
272.5O.273.s01 MS
Lod0l
Lodol
o
o
o
o
NL:0
tf'lz=282.8-2U.3Fi -c
ESI SRM ms2
303.20@15.00 [
2A2.75-2U.251 MS
Lod0'l
fime (min)
02l1aa7 12'.45'.27
100 ppm EDTA
'\eu
I
ftill=272.1273.5F: - c
ESI SRM ms2
291.20@15
r5.00 I
246.56247.fi,
246.50-247
272.5e273.s01 MS
:5.26E4
nlz= 246.5-247.5F: - c
rn/z= 325.5-326.5 F: - c
ESI SRM ms2
344.20@1s.00 [
299.50.300.50,
325.50-326.501 MS
Lod02
ESI SRM ms2

2s1.20@15.00 I
246.50-247.50,
272.s0.273.501 MS
Lod02
o
o
o
NL:4.66E3
: E.16E3
311 .5-312.5 F: - c
ESI SRM ms2
356.00@15.00 I
31 1.50.312.501 MS
Lod02
nlz=282.8-2U.3 F: - c
ESI SRM ms2
303.20@15.00 t[
282J2$284.251 MS
nlz=
6u,/,
(t-ts
Time (min)
0211207 12:49:20
100 ppm EDTA
T,F
NL:6.6585
mlz= 272.5-273.5F: - c
ESI SRM hs2
291.20@15.00 I
246.50-247.50,
272.50-273.501 MS
Lod03
t*r
--l
*-l
*.]
*-l
Lod03
NL:4.28E4
rnlz= 246.5-247 .5 F: - c
ESI SRM ms2
291.20@15.00 [
246.50-247.50,
272.s0-273.501 MS
Lod03
?o-l
"1
,8 60l
^-l
--l
so-]
nlz=282.8-2U,3F:.
ESI SRM msZ
30320@1s.00 [
282J3$284.251 MS
al
s0-l
"l
ro-1
,l
60-l
--l
*.]
50-J
ou-]
I
oo-l
*-l
6rw
(a
sc.
ESI SRM ms2

344.20@15.00
299.5G300.50.
F: -
325.50-326.50} MS
7sJ
1001
n/z= 299.5-300.5
02h207 12:53:15
C:Xcalibur\...\LOD_Negati
50 ppm EDTA
NL:2.32E4
NL:4.19E4
ntlz=272.*273.5
'TPP
F: -
rnlz= 299.5-300.5 F: . c
ESI SRM ms2
344.20@15.001
,qo qo-?no qn
ESI SRM ms2

291.20@15.00 [
246.50-247.50,
272.50-273.s01 MS
LodOl
325.50-326.501 MS
Lod04
:3.31E3
10(
r/z= 325.$326.5
F: - c
ESI SRM ms2
ESI SRM ms2
29120@1s.00 [
344.20@1s.oo I
299.50-300.50.
325.50-326.501 MS
LodOl
246.fi-247.50,
272.s0-273.501 MS
Lod04
8(
7l
7(
ba
Qar
e
@
-c
3,41E3
mlz=282.8-2U.3F: - c
r/z= 311.$312.5
ESI SRM ms2

303.20@15.00 [
ESI SRM ms2

356.00@1s.00
282.75-2u.251 MS
311.50-312.s0j MS
Lod04
Lod04
E,v
1.5
Time (min)
F: - c
C:l(calibur\...\LOD_Negativ
02fi407 12:57:07
50 ppm EDTA
joP
NL:1.34E4
mlz=272.5-273.5 Fi - c
0.77
ESI SRM ms2

291.20@15.00 [
246.&-247.50,
272.50-273.501 MS
Lod05
NL:'1.77E3
r/z= 325.5-326.5 F: . c
'r'lz= 246.5-247 .5 F: - c
ESI SRM ms2
291.20@15.00 [
246.50-247.50,
272.5C273.sO1 MS
Lod05
ESI SRM ms2
344.20@1s.00 {
299.50-300.50,
325.50-326.501 MS
LodO5
NL:0
NL: 6.90E3
rnlz:- 282.V2U.3 F: - c
ESI SRM ms2
303.20@15.00 [
282.75-2u.251 MS
Lod05
rn/z=311.5-312.5
&
Time (min)
F:.c
ESI SRM ms2
356.00@1s.00 [
311.50-312.501 MS
Lod05
vq,
Time (min)
C :U(ca
libuA...\LOO-Nesativ6';b
0?J12107 01 :01:00
50 ppm EDTA
')pt'
NL:4.54E5
rtlz= 272.5-273.5 F: - c
o0l
ESI SRM m9
291.20@15.001
--l
246.9-247.50,
^.1
272.50-273.s01 MS
Lod06
7.54E3
nr/z= 325.$326.5 F: - c
ESI SRM ms2
344.20@15.00 [
299.50-300.50.
325.50-326.501 MS
Lod06
ftlz=246.5-247.5 F: - c
ESI SRM msz
29120@15,00 [
246.50-247.fi.
272.50.273.501 MS
Lod06
.E
10(
r/z= 311.5-312.5 F: - c
ESI SRM ms2
356.00@15.00 [
311.s0-312.501 MS
Lod06
8:
EO
7C
6C
55
40
30
Time tminl
bD
1.5
nme (min)
C :U(calib
ur\...\LO O-f.f
0211A07 01:04:53
"Orr'@
100-t
*l
oJ
-J
ESI SRM ms2

291.20@15.00 [
246.50-247.50,
272.50-273.501 MS
25 ppm EDTA
NL: 1.63E4
miz= 299.5.300.5 F: . c
ESI SRM ms2
344.20@15.001
299.50-300.50,
325.50-326.501 MS
Lod07
NL:123E4
246.5-247 .5 F: - c
']/z=SRM msz
ESI
291.20@15.00 [
248.50-247.50,
272.50-273.501 MS
Lod07
NL:1.79E3
nlz= 282.8-2U.3 F: - c
ESI SRM ms2
303.20@15.00 I
282.7$284.251 MS
Lod07
r/z=
325.5-326.5 F: - c
ESI SRM ms2
344.20@15.001
299.50.300.50,
325.50-326.50t MS
Lod07
rvz= 311.5-312.5 F: . c
ESI SRM ms2
356.00@15.001
311-5O312.501 MS
02J12107 01:08:47
25 ppm EDTA
NL:1.27E4
nvz= 299.5-300.5 F: - c
ESI SRM ms2
344.20@15.00 I
299.50-300.50.
325.50-326.50t MS
Lod08
1001
NL:1.10E4
1z.246,5-247.5F:-c
ESI SRM msz

29'1.20@15.001 [
2e1.20@15.00
".]
246.50-247.50,
272.s0-273.501 MS
s5-l
299.50-300.50,325.50-326.501 MS
Lod08
8J
?l
?0-l
ari
ffVz= 325.5-326.5 F:
ESI SRM ms2
344.20@15.00 t
60--l
f,y 4+b
Gt)
-c
0211A07 01:12:45
NL:2.03E5
nlz--272,5-273.5F: - c
25 ppm EDTA
NL:2.44E4
m/z= 299.5-300.5 F: - c
ESI SRM msz
ESI SRM ms2

291,20@15.00 [
344.20@1s.00 [
246.50-247.50.
299.50-300.50.
272.50-273.501 MS
Lod09
325.50-326.s0t Ms
Lod09
rn/z= 325.5-326.5 F: - c
ESI SRM ms2
344.20@15.00 [
299.50-300.50,
325.50-326.501 MS
Lod09
I
o
e
!o
4.73E3
t00
90
AE.
E0.
65.
60.
555U-
4540-
3$
30-
[+ a(
( tta
C :U(ca
libur\...\LOD-NeSati{11E
0.77
0U12107 01:16:37
NLi 4.42E4
'll/z= 272.5-273.5 F: - c
ESI SRM ms2
291.20@15.00 I
246.50-247.50,
272.50-273.501 MS
Lod10
13 ppm EDTA
atF
NL:2.'13E4
m/z= 299.5-300.5 F
ESI SRM ms2
344.20@15.00 I
299.50-300.50,'
325.50-326.50t MS
Lod'10
r'lz=246.+247.5F:. c
ESI SRM ms2
291.20@15.00 [
246.50-247.50,
272.50-273.501 MS
Lod10
o
o
d
:
o
NL: 0
tnlz=282.8-2g.3 F: - c
ESI SRM ms2
303.20@15.00 [
282.752U.251 MS
Lod10
f+ q(
(zst)
8.91E2
m/z= 3'11.$312.5 F: . c
ESI SRM ms2
3s6.00@15.00 [
311.50-312.501 MS
02112107 01:20:32
13 ppm EDTA
Jtg
NL:6,86E4
rniz=272.5-273.5 Fi - c
ESI SRM ms2
291 .20@15.00 [
246.50-247.50.
272.50-273.s01 MS
:9.E7E3
1.00E4
m/z= 325.5-326.5 F: . c
ESI SRM ms2
344.20@15.00 [
299.50.300.50.
325.50-326.501 MS
f,]lz=246.5-247.5 F: - c
ESI SRM ms2
291.20@15.00 [
246.50-247.50,
272.50-273.s01 MS
Lodl I
Lodll
o
d
o
@
fEDTfjronl
.tlz=282.8-2U.3
F'.
-c
ESI SRM ms2

303.20@15.00 [
282.75-28/.251 MS
Lodt'l
tr
qq
( ts+
r r1tra
rvz=
3 l 1.5-31 2.5 F: - c
ESI SRM msz
3s6,00@15.00 I
3'11.50-3'12.501
Lodl
MS
0?i1?i07 01:24:25
13 ppm EDTA
NL:8.62E4
NL: 1,76E4
nr/z= 299.5-300.5
ESI SRM ms2
344.20@1s.00 [
nlz=272.5-273.5 F: - c
ESI SRM ms2
291.20@15.00 [
246.50-247.50,
272.50.273.501 MS
Lod12
F: . c
299.50.300.50,
325.50-326.501 MS
Lodl2
:5.86E3
rnlz=246.*247.5 F: - c
r/z= 325.S326.5 F: - c
ESI SRM ms2

291.20@15.00 [
ESI SRM ms2
34420@1s.00 [
246.50-247.9,
299.50-300.50,
325.50-326.501 MS
Lod12
272.s0-273.501 MS
Lod12
8
f,
o
.g
NL:2.45E3
rfllz=282.*2U.3 Fi - c
r/z=
ESI SRM ms2
ESI SRM ms2
303.20@1s.00 [
356.00@15.00 [
311.50-312.501 MS
282Js-2U.251 MS
31
Lod'12
Cv qv
( 3ss
1.5
Time (min)
1.5
Time (min)
2.0
1.''312.5 F: - c
02112107 01:28:18
6 ppm EDTA
r/z= 299.5-300.5
F: - c
ESI SRM ms2

344.20@15.00
r5.00 [[
299.50-300.50,
325.50-326.501 MS
Lod13
00-l
'l
nvz= 325.5-326.5 F: - c
ESI SRM ms2
^-l
s0J
^-l
;;l
344.20@15.00 I
299.50-500.50,'
325.50-326.50t MS
Lodl 3
?5-]
I
to-1
uuJ
m/z= 31 1.5-312.5 F: . c
ESI SRM ms2
3s6.00@15.00 [
311.50-312.50) MS
Lodl 3
0?/1?./07 01:32:10
6 ppm EDTA
NL:2.77E4
nlz=272.$273.5 F: - c
ESI SRM ms2
291.20@15.00 I
246.50-247.50,
34420@1s.00
272.50-273.50t MS
Lod'14
1001
*l
n<--l
Lod 14
ro-l
75-..1
7o-.1
*l
I-l
60-]
1.66E3
(r|F282.8-2U.3F:
-c
ESI SRM ms2

303.20@15.00 [
282-752U.251 MS
Lod14
tr.+,1,
( )s't
l'lme (min)
299.50-300.50,
325.50-326.501 MS
Lodl4
mlz= 246.*247.5 F: - c
ESI SRM ms2
291.20@1s.00 [
246.50.247.50.
272.50-273.50t MS
"-l
s0-1
m/z= 299.5-300.5 F: - c
ESI SRM ms2
NL:2.75E3
r/z=
325.S.326.5 F: - c
ESI SRM msz
3rf4.20@15.00 [
299.50-300.50,
325.50-326.s01 MS
Lod14
C:U(calibur\...\LOD
,::
6 ppm EDTA
0211207 01:36:03
NL: 3.67E4
NL:5.92E3
nlz=272.5-273.5Fl- c
rvz= 299.5-300.5 F: - c
ESI SRM ms2
::l
JhP
ESI SRM ms2
291.20@1s.00 [
246.50.247.50,
344.20@15.00 [
299.50.300.50.
272.5&.273.501 MS
Lod15
325.s0-U6.501 Ms
Lodl 5
4.80E3
rvz= 325.S326.5 F: . c
ESI SRM ms2
344.20@15.001
299.50.300.50.
325.50-326.501 MS
Lodl5
o
6
NL:4.72E3
trVz= 31 1.t312.5 F: ESI SRM ms2
3s6.00@15.00 [
311.50-312.501 MS
Lod15
0.53
&-,/w
338
/\
tl
Seq uence--LOD2_neg. sld [Open]

C--nent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
LOD16
05
C:Xcalibur\Data\EDTA\Brewer\LOD Neoative G:Xcalibur\methods\EDTA Nec
Proc Method
CalFile
Position
InjVol
b.u
Sample Name:
Inst Method
Level
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
u.00u
ppm
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Proc Method
CalFile
Position
InjVol
5.0
Level
tH*****s******t*it**********************t*****************i*********************************t***ff**********
r q(u
( 3)q)
page
7*V
p\r,\'1
Sequence--LOD2_neg. sld [Open]

C^nment:
Study:
Client:
Laboratory:
Company:
Phone:
Proc Method
GalFile
Position
InjVol
5.0
Level
Sample Wt
Sample Vol
ISTD Amt
0.000
u.000
0.000
***********t**************t***********************************************i*t*+*********i*****t**************t******************************r**
Sample Name:
.6 ppm EDTA
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Unknown
LOD19
05
Proc Method
Cal File
Position
InjVol
5.0
Path
Inst Method
:\Xcall bur\Data\E DTA\Brewer\LO D_Negative
Level
:\Xcallbur\methods\EDTA Nec
Sample Wt
Sample
0.000
0.000
Vol
IISTD Amr
0.000
{n rl,lu
( l+r)
page 2
5rl
1Pto1
Sequence--LOD2_neg. sld [Open]

Sample Name: 1.6 ppm EDTA
C'-"nent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Unknown
LOD2O
05
Proc Method
Cal File
Position
.,
t
Path
Method
:Xcalibu AData\EDTA\B reweALO D_Negative C:U(calibuAmethods\EDTA Neo

lnjVol
Level
b.0
Sample Wt
Sample Vol
ISTD Amt
rJ.{J00
0.000
0.000
*******************s***i*******************i*************t*****************
Sample Name: 1.6 ppm EDTA

Comment:
Study:
Client:
Laboratory:
Company:
Phone:

Unknown
LoD21
Proc Method
CalFile
Sample lD
105
Path
C
lnst Method
:\)(cali bu r\Data\EDTA\Brewer\LO D_N eg ative C:Xcalibur\methods\EDTA Neq
Position
InjVol
5.0
Level
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
U.UUU
arV
a
ht-,/-VVb
\
()ar\
nana ?
'/
'Lltv\'t
02112107 01;46:39
r]/z=272.1273.5Fi - c
ESI SRM ms2
291 .20@15.00 [
246.50-247.50,
272.s0r73.501 Ms
1001
ru-l
*.1
851
NL: 1.83E3
'n/z= 246.1247 .5 F: - c
ESI SRM msz
2e1.20@15.001
246.50-247.50,
272.50273.501 MS
*.]
?l
7q
.*l
60-l
r00l
ru-J
*-l
8q
filz= 282.8-2U.3F..
ESI SRM ms2
303.20@15.00 I
-c
282.75-2U.251 MS
Lod'16
8o-l
tr-l
'o-l
6l
60-]
--
"rl
rol
oul
oo'1
,.]
{*a4
G4j
NL:0
fil/z= 299.5-300.5 F: - c
ESI SRM ms2
344.20@15.00 I
299.50.300.50,-
32s.50-326.501 MS
Lod16
325.5-326.5 F: - c
ESI SRM ms2
344.20@15.00 r
299.50-5oo.so.'
325.s0-326.501 MS
'
C:U(calibuA...\LOD
02l1VO7 01:50:58
3 ppm EDTA
NL:3.59E3
nvz= 299.5-300.5 F: - c
ESI SRM msz
u4.20@15.ooI
299.50.300.50.
325.50-326.501 MS
Lod17
nlz= 246.$247 .5 F: - c
ESI SRM msz
2s1.20@15.00 [
246.50-247.50.
272.50-273.501 MS
Lodl 7
o
-g
t7]lz=
282.8-2U.3 F: - c
ESI SRM ms2

303.20@1s.00 [
282.7$284.251 MS
LodlT
o'/'lU
(
t+)
C:XcalibuA...\LOD
0?J12107 01:54:50
NL:
nlz= 272.5-273.5 F: .
ESI SRM ms2

291.20@15.00 [
246.50-247.50.
272.50-273.501 MS
Lod18
1.90E3
246.5-247.5 F: - c
ESI SRM ms2
r!z=
2s1.20@1s.00 [
246.&-247.50,
272.50-273.501 MS
Lod'l
o
o
tn'/4b
( z+'\
3 ppm EDTA
0A12107 01:58:43
1.F ppm EDTA

NL: 1.23E3
m/z= 299.5-300.5 Fi - c
ESI SRM ms2
344,20@1s.001
299.50-300.50,
325.50-326.501 MS
Lodl 9
3.50E3
.5 Ft - c
ESI SRM ms2
291.20@15.00 I
246.5G247.50,
272.50.273.s01 MS
rn/z= 325.5-326.5 F: - c
ESI SRM ms2
lod19
Lod19
nlz= 246.*247
344.20@15.00 [
299.50-300.50,
325.50-326.501 MS
NL:
: 1 .35E3
n{z=282.V284.37: - c
r/z=
ESI SRM msz

303.20@15.00 [
282.7$.284251 MS
ESI SRM ms2

356.00@15.00 [
311.50-312.50j MS
Lod'19
Lod'19
Lr
,
0.0
-dl,+DTFfi?A
0.s
1.0
1:5
Time (min)
2.0
2.5
3.0
q"(
( *s)
Time (mrn)
31 1.5-312.5 F: - c
02112107 02:02:36
C:U(calibur\...\LOD_
1.6 ppm EDTA
NL: 1.98E3
nriz= 299.5-300.5 F: - c
ESI SRM MS2
344.20@1s.00 I
299.5C300.50,
325.s0-326.501 MS
Lod20
NL: 5.20E3
.r/z= 272,5-273.5 F: - c
100-l
'ESl SRM ms2
'
-"1-
291.20@15.00 [
246.50-247.50,
272.50-273.501 MS
Lod20
.r.lz=2465-247.5 Fi - c
m/z= 325.+326.5 F: - c
ESI SRM ms2
344.20@15.00 {
299.50-300.50,
325.50-326.501 MS
Lod20
ESI SRM ms2

291.20@15.00 [
246.50-247.50.
272.50-273.501 MS
Lod20
ud
e
o
-s!
nlz= 282.8-2a43
F'.
-c
ESI SRM ms2

30320@15.0O I
282.75-284251 MS
Lod20
fn qva
( z+)
Tlme (min)
-l-oF
Trme (min)
'
:Xca I ibu r\...tt-O
RT:03d100-l
ss-]
I
'n-l
O-N.g"tir6f;2l
0A1UO7 02:06:29
1.6 ppm EDTA
'f
rpP
3o-5
0.77
NL: 2.81 E3
rtlz= 272.5-273.5 F: - c
rn/z= 299.$300.5 F: ESI SRM ms2

34420@15.00 I
ESI SRM ms2
291.20@15.00 [
246.50-247.50,
272.50-273.501 MS
299.50-300.50,
325.50-326.501 MS
Lod21
Lod21
nJz= ?46.5-247.5 F: ESI SRM ms2

291 .20@15.00
rvz= 325.5-326.5 F: - c
ESI SRM ms2

34420@15.00 [
299.50-300.50,
325.50.326.501 MS
246.50-247.50,
272.50-273.501 MS
Lod2l
Lod21
o
o
100-
v590-
fi1lz=282.8-2U3 F: - c
ESI SRM ms2
303.20@1s.00 [
282.75-2U.251 M8
Lod2l
858075-
605J-
s45-
403530-
{* aqG
rrz:
31 1 .5-3'12.5 F: - c
ESI SRM ms2
356.00@15.00 [
311,5S312.501 MS
Sequence--LOD_pos. sld [Open]

Sample Name: 100 ppm
C-
rent:
Study:
Client:
Laboratory:
Company:
Phone:
Samole lD
Path
Unknown
LODOl
Proc Method CalFile
Position
1
lnst Method
:Xcalibur\Data\EDTA\Brewer\LOD Positive
nJvol
Level
5.0
:Xcalibur\methods\EDTA Pos
Samole Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000

Study:
Comment:
Client:
Laboratory:
Company:
Phone:
Sample Type
Unknown
ile Name
LODO2
lnst Method
Sample lD
Path
01
C:U(calibur\Data\EDTA\Brewer\LOD
Position
InjVol
5.0
Level
Positive C:U(calibur\methods\EDTA Pos
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
t**********i*************t*******i****************tf****t***t********t*t*****t*#**************tl
{rc (,t c'

(
vt)
1
ft'
>lr-1"'1
Seq uence---LoD_pos. sld [OpenJ

Sample Name: 100 ppm EDT
C-
'.nent:
Study:
Client:
Laboratory:
Company:
Phone:
Samole lD
Path
Unknown
LODO3
01
C:Xcalibur\Data\EDTffi
Proc Method
CalFile
Position
InjVol
5.0
Level
Inst Method
C:Xcalibur\methods\EDTA pos
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
******ti*****************i********t******t***t*********************
Sample Name:
ppm ED
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Proc Method
CalFile
Position
InjVol
5.0
Level
Sample Wt
Sample Vol
0.000
0.000
Amt
0.000
****t*******************************t*************r******
{r avu
(t+';
:Ts
tlvi."t
Seq uence---LO D_pos. sld [Open]

Sample Name:
(-
nent
rl
Study:
Client:
Laboratory:
Company:
Phone:
C:Xcalibur\metnoOs\eDTR
***t*t***********************************************i*t************************t***********************t**************************t******l**t*
Sample Name:
Comment:
ppm EDT
Study:
Client:
Laboratory:
Company:
Phone:
**8**t******************t***************************************************************#***********i*********i*******t**r*************i***
[y +qb
( zs')
JOF
Llttlc
Sequence---LOD_pos. sld [Open]

Study:
nent:
Client:
Laboratory:
Company:
Phone:
lnst Method
Sample lD
Path
Unknown
LODOT
03
C:Xcalibur\Data\EDTA\Brewer\LOD Positive C:U(calibur\methods\EDTA Pos
Proc Method
Cal File
Position
lnjVol
5.0
Level
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
**f *********tr*******t
*******tl*************ii*******ff
Sample Name: 25 ppm

Study:
Comment:
Client:
Laboratory:
Company:
Phone:
lnst Method
Sample lD
Path
Unknown
LODOS
)4
C:Xcalibur\Data\EDTA\Brewer\LOD Positive C:Xcalibur\methods\EDTA Pos
Proc Method
Cal
File
lPosition
InjVol
Level
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
5.0
t***t**t*********************l******
fr
qqc'
ArF
'ultl"'7
Seq uence--LOD_pos. sld [Open]

C- 'nent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
LODOg
03
C:Xcalibur\Data\EDTA\Brewer\LOD Positive C:U(calibur\methods\EDTA
Proc Method
Cal File
Position
InjVol
5.0
Inst Method
Level
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0,000
Pos

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
04
C:Xcalibu r\Data\EDTA\Brewer\LOD Positive C:U(calibur\methods\EDTA Pos
Position
InjVol
5.0
oD10
Inst Method
Level
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
*************t
fo'/u,
(st^)
oaoe 5
Jb!
uf vf "t

Sample Name: 13 ppm
C-
'.nent:
Study:
Client:
Laboratory:
Company:
Phone:
lnst Method
Sample lD
Path
Unknown
LOD11
04
C:Xcalibur\Data\EDTA\Brewer\LOD Positive C:Xcalibur\methods\EDTA
Proc Method
CalFile
Position
InjVol
5.0
Level
Sample Wt
Samole Vol
ISTD Amt
0.000
0.000
0.000
Pos
**t*****t*******************i**************t***********t**t*******
Sample Name: 13 ppm E

Study:
Comment:
Client:
Laboratory:
Company:
Phone:

Unknown
LOD12
Proc Method
Cal
File
lnst Method
Sample lD
Path
04
C:XcalibuAData\EDTA\Brewer\LOD Positive C:Xcalibur\methods\EDTA
iPosition
InjVol
5.0
Level
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
Pos
**********t*t********************************i***********
tn u+o
( zs)
nana A
Jrf
Llvl"1

rent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Unknown
LOD13
05
Proc Method
Cal File
Position
InjVol
5.0
Path
Inst Method
:U(calibuAData\EDTA\BreweALOD Positive
Level
:U(calibur\methods\EDTA Pos
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
***t*****************

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
LOD14
05
C:\)(calibur\Data\EDTA\BreweALOD
Proc Method
Cal File
Position
InjVol
5.0
Inst Method
Level
Positive
:U(calibur\methods\EDTA Pos
Sample Wt
Samole Vol
ISTD Amt
0.000
0.000
0.000
***********************************t*t******l*******************t**************************
{'*
ou
( zs+)
aaaa'7
J DI'
-,n
'L II
ItLl2
Sequence---LoD_pos. sld [Open]

nent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
LOD15
05
C:U(calibuAData\EDTA\BreweALOD Positive C:U(calibuAmethods\EDTA Pos
Proc Method
Cal File
Position
InjVol
5.0
Inst Method
Level
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
u : \xcal tbu r\uata\tsLJ I A\H rewer\Lu
Unknown
LOD16
UO
Proc Method
Cal File
Position
njVol
Inst Method
Level
5.0
fr. uuo
( zs)
Postttve C:U(calibur\methods\EDTA Pos
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
JbF
t lwbt

Sample Name:
ppm EDTA
-nent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
LOD17
06
Proc Method
Cal File
Position
InjVol
5.0
Inst Method
Level
Positive C:U(calibur\methods\EDTA Pos
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
*****************t*****s*tr*t*********i******************tt**t**t*i********t**********s*******t***r*******ti*********t***********r***********

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
sampre rype File Narne
Sample lD
Path
lnst Method
Unknown
LOD18
06
C:Xcalibur\Data\EDTA\Brewer\LOD Positive C:Xcalibur\methods\EDTA Pos
Proc Method
Cal File
Position
InjVol
Level
5.0
f'r aqb
( es)
nana
Sample Wt
Samole Vol
ISTD Amt
0.uuu
0.000
0.000
'Jrf
rlvl"t

Sample Na
(-
1.6 ppm EDTA
nent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
LOD19
07
C:UKcalibur\Data\EDTA\BreweALOD Positive C:U(calibur\methods\EDTA Pos
Proc Method
CalFile
Position
InjVol
5.0
Inst Method
Level
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
Sample Name: 1.6 ppm

Study:
Comment:
Client:
Laboratory:
Company:
Phone:
Inst Method
Sample lD
Path
Unknown
LOD2O
07
Proc Method
Cal File
Position
njVol
Level
5.0
fr'/'/('
(
zst)
Positive C:\)(calibur\methods\EDTA Pos
Sample Wt
Sample Vol
0.000
0.000
ISTD Amt
10.000
{bF
,lrr-lo1
Sequence---LOD_pos.sld [Open]
Sample Name:
.6 ppm EDTA
Study:
-rent:
Client:
Laboratory:
Company:
Phone:
Sample Type File
Name lSample lD
lnst Method
Path
Unknown
LOD21
07
C:U(calibur\Data\EDTA\BreweALOD Positive C:Xcalibur\methods\EDTA Pos
Proc Method
Cal File
Position
InjVol
5.0
Level
{r 4ab
( zst)
Sample Wt
Sample Vol
ISTD Amt
0.000
0.000
0.000
tr
,11'l
.C:\)(calibuA...\LOD_Positive\Lod01
02112107 02:43:57
100 ppm EDTA
101#60 RT: O.81 AV:
1001
NL:4.04E5
rVz= 159.5-160.5
F: + c ESI Full msz
'-t
293.00@1s.001
125.00-315.001 MS
Lod01
1001
F: + c ESI Full ms2

293.00@15.00 [
r25.00-315.001 Ms
Lod0l
vvl
ro-]
*l
*l
nnl
75-..1
I
701
^-l
fl
ao-.1
I
: 5.47E5
TIC MS Lod01
(-{
( ts'i
NL:4.55E5
+ c ESI Full ms2 293.00@15.00 [ 125.00-315.00]
t-ltF
02112/07 02:47:51
C :U(calibur\...\LOD_Positiveld02-
+ c ESI Full ms2 293.00@'15.00 [125.00-315.00]
NL:4.16E5
rol
nYz= 159.5.160.5
F: + c ESI Full ms2
293.00@15.001
125.00-315.001 MS
Lod02
*I
NL:5.06E5
TIC MS Lod02
IG
205
2.80
2.6
t"
'l
( eL,i
Time (min)
100 ppm EDTA
1001
ru-l
*-l
*t
AE.]
'l
'l
'l6l
o
,1 ^^l
,ol
'u-]
'o-]
*-l
'l
7ff
..]
uu-]
60-l
*.]
5o-l z
I 0.08
45_1
4/1il
'lll
C:\)(calibuA...\LOD_Positive\Lod04
02l1AO7 02:55:29
50 oom EDTA
tu4*i6 Kt: u./6 Av:1
NL: b.ZUE4
+ c ESI Full ms2 293.00@15.00 [125.00-315.00]
NL:3.76E4
rniz= 159.$160.5
F: + c ESI Full ms2
293.00@15.00 [
125.0G315.001 MS
Lod04
o
o
6
o
o
=d
o
l.zEEi
TIC MS Lod04
76
80
1.06
l
I
(o uu,
( zuz
C:U(calibuA...\LOD_Positive\Lod05
02112107 02:59:15
NL:8.6'1E4
rn/z= 159.$160.5
F: + c ESI Full ms2
293.00@1s.00 I
12s.00.315.001 Ms
Lod05
65N-
4540-
zb
20't510-
: 1.00E4
trtlz- 246.5-247 .5
F: + c ESI Full ms2

293.00@1s.oo I
't25.00-3'15.001 MS
LMUS
t,a
(tat
+ c ESI Full msz 293.00@15.00 [ 125.00-315.00]
:U(calibuA...\LOD_Positive\Lod06
0211i/07 03:03:06
50 ppm EDTA
a---
1 NL:
+ c ESI Fullhs2 293.00@15.00
[125.00-315.001
160
NL:5.82E4
1OGr
'l
^-l
,ol
*-l
rn/z= 159.5-160.5
F: + c ESI Full rnsz
293.00@15.00 [
125.00-3'15.001 Ms
Lod06
1.42E4
F: + c ESI Full ms2
293.00@15.00 [
125.00-315.001 MS
Lod06
ru-]
*t
ao!
tr-l
1l
o"-'l
,'1
oo
f
E
o
o
o
x,
NL:2.40E5
TIC MS Lod06
{oqu
(
:\)(calibu r\...\LOD_Positive\LodO7-
02112107 03:06:59
25 ppm
EDTA
RT: 0.00
: + c ESI Full ms2 293.00@15.00 [ 125.00-315.001

1
0.85
00-l
*l
9.40E3
nlz= 246.U247.5
F: + c ESI Full ms2

293.00@15.00 [
125.00-315.001 MS
Lodo7
o
o
6
!
o
.z
o
o
NL: 1.99E5
TIC MS Lod07
43
0.71
ta
0.33
1.5
Time {min)
:U(calibuA...\LOD_Positive\Lod09,
'ol
*l
0212/07 03:14:36
luvRiz Kt: u.64 Av: I NL: 2.ZtE4
NL: 1,69E4
rn/z= 159.$160.5
F: c ESI Full msz
293.00@15.00 [
12s.0G315.001 MS
Lod09
+ c ESI Full ms2 293.00@15.00 125.00-315.00]

[
4.42E3
1001
ru-]
*-l
tr'lz= 246.5-247 .5
F: + c ESI Full ms2
293.00@15.00 [
12s.00-315.001 Ms
,u-]
*l
FAJ
75-i
to-]
--t
^J
o
o
6
P 'nl
4
o
6
rrc us r-oaos
j.!2,
-NL:2.18E5
fo,l,l
1001
,5-l
*-1
2.01E3
rnlz= 246.*247 .5
F: i c ESI Full ms2
293.00@15.00 [
125.00-3't5.001 MS
Lod08
8s-l
'o-l
tu-l
7o--l
.']
to
q+
(r"l
c ESI Full ms2 293.00@15.00 [ 125.00-315.00]
C:\)(calibuA...\LOD_Positive\Lod 1 0
od10*r61 RT: 0.83 AV:
NL: 3.45E4
: + c ESI Full ms2 293.00@15.00 [ 125.00-315.00]
,:l
"l
5 qatra
rilz= 246.*247
.5
F: c ESI Full ms2

293.00@1s.001
125.00-3'15.001 Ms
Lodl 0
*J
*l
rnJ
--l
zs--l
I
toJ
*l
I
{,^t +'l t"
(tus)
:l(calibur\...\LOD_Positive\Lod
1 1
0A1ZO7 03:22:11
NL: 1.89E4
m/F 159.$160.5
F: + c ESI Full ms2
293.00@15.00 [
125.00.315.001 MS
Lodl
t*-]
*l
*.1
*.1
NF246.5-247.5
t"a
F: + c 551 Pr1
293.00@15.00 [
125.0C315.001 MS
Lodi 1
80-l
7s-l
,0-l
"
':-]
[+ aau
( 2,,,q\
+ c ESI Fult ms2 293.00@15.00 125.00-315.00J

[
C:\)(calibuA...\LOD Positive\Lod12
13 ppm EDTA
0?/12107 03:26:02
0d1?#61 Rl:0.E3 AV:1 NL:2.42E4

: + c ESI Full ms2 293.00@15.00 [ 125.00-315.001
00-l
I
s5-1
""-l
nlz= 246.$247.5
F: + c ESI Full ms2
293.00@15.00 I
125.00-315.00t MS
Lod12
AqJ
--t
*l
nnJ
ru-l
70-J
I
ai-J
--l
P -l
o
6
tr
z.ocE3
TIC
MS Lodl2
f,r 4,tb
ar
i4
C:XcalibuA...\LOD Positive\Lod 1 3
02112107
03:29:50
l'13#63
or.
NL:1.03E4
n/z= 159.$160.5
64
0.87
F: + c ESI Full msz

293.00@15.oo l
125.00-315.001 Ms
Lod13
227E3
n|F246.1247.5
F: + c E6l Full ms2
293.00@15.00 |
125.00.315.001 MS
Lod13
NL:2.31E5
TIC MS Lod13
t.3
6 ppm EDTA
t{l: u.65 AV: I
NL: J.zbE4
+ c ESI Full ms2 293.00@15.00 [125.00-315.001
:U(calibur\...\LOD_Positive\Lod
02112107 03:33:39
NL; 1.29E4
n/z= 159.F160.5
F: + c ESI Full ms2
293.00@15.001
125.00-315.001 MS
Lod14
1001
rnlz= 246.5-247.5
F: + c ESI Full ms2
293.00@15.001
125.00-315.001 MS
Lod14
*.]
*-l
'l
to'1
--l
o -.-t
1
:2.46E5
TIC MS Lod 14
tn,tu,
( tt,t
0?/1U07 03:37:26
NL:'1.91E4
rvz= 15S.5-160.5
F: + c ESI Full ms2
293.00@1s.00 [
125.00-315.001 MS
Lod15
':l
"l
*l
*l
rol
'l
7H
.c
"-l
^^l
-t
ty aau
(
ztz
+ c ESI Full ms2 293.00@15.00 [ 125.00-315.001
C:U(calibur\...\LOD_Positive\Lod
0?J12107 03:41:16
NL: 2.31 E4
100-r
I
--l
Full ms2 293.00@15.00 [ 125.00-315.00]
nvz= 'l 59.5-1 60.5

F: + c ESI Fult ms2
293.00@1s.00 [
125.00-315.001 MS
Lodl 6
fttlz= 246,5-247.5
F: + c ESI Full ms2
293.00@15.00 [
125.00-315.001 MS
Lod16
o
o
o
f
o
.c
2.27E5
TIC
MS Lodl6
t*
qqo
n+)
3 ppm EDTA
C:U(calibuA...\LOD Positive\Lod 1 7
02112/07 03:45:05
3 ppm EDTA
+ c ESt Fuil ms2 293.00@15.00 125.00-315.00]

[
--
2.78
rnlz= 246.5-247.5
F: + c ESI Full ms2
293.00@1s.00 [
125.00-315.001 MS
o
o
6
of
o
6
E,
166
TIC
2.01E5
MS Lod17
2.26
263
fr
(
qo
tts
:U(calibuA...\LOD_Positive\Lod
041U07 03:48:52
NL:7.78E3
':i
+ c ESI Full ms2 293.00@15.00

[125.00-315.001
rnlz= 159.5-'160.5
F: + c ESI Full msz
2s3.00@1s.00 [
125.00-315.001 MS
LodlS
1001
rul
el
*l
l.l3E3
ft/z=246.5-247.5
F: r c ESI Full ms2

293.00@15.00 [
125.00-315.001 MS
Lodl
*-l
ru-l
to-]
"
6l
o
o
-n-l
!
oa
o
o
6
E.
'NL:229E5
TIC MS Lod18
{r,1,1
( z'tu
3 ppm EDTA
MATRIX
fo vqu
( ztt)
Seq uence---MATRIX_pos. sld [O pen]
.0
("50 ppm")
Sample Name:
-ment:
Study:
Client:
Laboratory:
Company:
Phone:

Unknown
MATRIXOl
Samole lD
I
Path
C
:\Xcalibu r\Data\E DTA\BreweAMAT Positive
Proc Method
lnst Method
CalFile

Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Sample Name:
Position
lnjVol
5.0
Samole Wt
Level
0.000
atrix
Study:
Comment:
Client:
'l-aboratory:
Company:
Phone:

Unknown
MATRIXOz
Samole lD
Path
02
C:Xcalibur\Data\EDTA\Brewer\MAT Positive
Proc Method
lnst Method
CalFile

Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Position
InjVol
5.0
Level
lSample Wt
0.000
************i
-..,tr(
f,* uo,;
I rts)
nana 'l
.Llpl.1
Sequence---MATRIX_pos. sld [Open]

Sample Name: Matrix 8 ("50 ppm")
C--rment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Unknown
03
MATRIXO3
Inst Method
Path
:XcalibuAData\EDTA\Brewer\MAT Positive
Proc Method
CalFile

Sample Vol
0.000
STD Amt
0.000
Position
InjVol
5.U
Sample Wt
Level
0.000
Dil Factor
1.000
*ff****t*****
9 ("50 ppm
Sample Name:
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
04
C:U(calibur\Data\EDTA\Brewer\MAT
MATRIXO4
lnst Method
Proc Method
CalFile
C:XcalibuAmethods\EDTA Pos
Samole Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Positive
Position
InjVol
5.0
Level
lSample Wt
0.000
*****************************t***********************t*************t***********************t*********t**************************************
/'
L4 +tlb
( )'11\
nana )
{q0
r lrr \:1
Seq uence---MATRIX_pos, sld [Open]

Sample Name: Makix 10 ("50 ppm")
f---rment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
05
C:U(calibuAData\EDTA\Brewer\MAT
MATRIXOS
Inst Method
Proc Method CalFile

Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Position
10
Positive
njVol
Sample Wt
Level
5.0
0.000

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
06
C:U(calibuAData\EDTA\Brewer\MAT
Inst
MATRIXO6
Method
Positive
iProc Method
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
{rP
f* *of( zs)
nana ?
r- lrr-\o1
Sequence--MATRIX_pos. sld [Open]

Sample Name:
ppm
C^"rment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
06
C:XcalibuAData\EDTA\Brewer\MAT Positive
MATRIXOT
Proc Method
lnst Method
Cal File

Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Position
lnjVol
12
5.0
Sample Wt
Level
0.000
****t**t*****t**********+*l*s*t***tt*********************t**

Study:
Comment:
Client
Laboratory:
Company:
Phone:

Unknown
MATRIXOS
Sample lD
Path
UO
C:U(calibur\Data\EDTA\BreweAMAT Positive
Proc Method
lnst Method
CalFile

Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
Position
InjVol
12
5.0
Sample Wt
Level
0.000
****t***t********s******t**********************************t***********
tu
4"0
+Vt"
( +s)
oaoe 4
Lf t- i"e

Sample Name:
/^-rment
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
06
C :U(cal ibu
MATRIXOg
lnst Method
Proc Method
r\Data\EDTA\Brewer\MAT Positive
CalFile

Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
Position
lnjVol
12
c.tJ
Level
Sample Wt
0.000

Gomment:
Study:
Client:
Laboratory:
Company:
Phone:

unKnown
MATRIXlO
Sample lD
12
lnst Method
Path
;:u(calrDur\Data\tsu I A\Hrewer\MA
Proc Method
CalFile

Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Posttve
Position
InjVol
12
5.0
Sample Wt
Level
0.000
*f ***********t*******
{+ a+u
lrse)
naoe 5
T'rP
1lt'\'r
Seq uence---MATR lX_pos. sld [Open]

.ment:
'
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
03
MATRIX13
Inst Method
:U(calibu r\Data\EDTA\Brewer\MAT Positive
Proc Method
Cal File
Position
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
I.UUU
njVol
Level
5.0
Sample Wt
U.UUO
Study:
Client:
Laboratory:
Company:
Phone:

Unknown
MATRIXl4
Sample lD
Path
o4
C:XcalibuAData\EDTA\Brewer\MAT Positive
Inst Method
Proc Method
CalFile
:Xcalibur\methods\EDTA Pos Swabs

Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Position
lnjVol
5.0
* qqo
(38,
aaaa
Level
Samole Wt
0.000
4ot
t\r'lJ
Seq uen ce---MATR|X_pos. sld [Open]

Sample Name: Matrix 5 ("500 ppm:')
c- rment:
Study:
Client:
Laboratory:
Company:
Phone:

Unknown
MATRIXlS
Sample lD
Path
06
C:Xcalibur\Data\EDTA\Brewer\MAT Positive
lnst Method
Proc Method
Cal File

Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
Position
InjVol
5.0
Level
Samole Wt
0.000
f ********************t*
Sample Name:
ppm EDTA
Comment:
Study:
Client:
Laboratory:
Company:
Phone:

Unknown
MATRIXl6
Sample lD
Path
06
C:XcalibuAData\EDTA\BreweAMAT Positive
lnst Method
Proc Method
Cal File
Position
InjVol
11
5.0
Level
iSamole Wt
I
u:\xcaltbunmetnods\EDIA Pos swabs

Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
V+to
( g?D
n:nc
0.000
5"0
r-
\rr'to'1

c-rment:
Study:
Client:
Laboratory:
Company:
Phone:

Unknown
MATRIXlT
Sample lD
Path
06
Proc Method
Inst Method
CalFile

Sample Vol
0.000
STD Amt
0.000
Positive
Position
InjVol
11
5.0
Sample Wt
Level
0.000
Dil Factor
1.000
*******i*********

Study:
Comment:
Client:
Laboratory:
Company:
Phone:

Unknown
MATRIXlS
Samole lD
Path
Ub
C:U(calibur\Data\EDTA\BreweAMAT
Proc Method
lnst Method
Position
Cal File
Positive
lnjVol
Level
Samole Wt
I

Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
11
tr +w( tss)
naoe 9
5.0
0.000
1n0
-t | ,4
.l \\
r\
^\.lt
b\
Seq uence---MATR lX_pos. sld [Open]
:"
Sample Name:
ppm EDTA
c'rment:
Study:
Client:
Laboratory:
Company:
Phone:

Unknown
MATRIXl9
Sample lD
Path
06
C:U(calibur\Data\EDTA\BreweAMAT
Inst Method
Proc Method
CalFile

Samole Vol
ISTD Amt
DilFactor
0.0u0
U.OOU
r.000
Positive
Position
lnjVol
11
5.0
Level
Sample Wt
U.UUU

Study:
Comment:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
06
MATRIX2O
Proc Method
lnst Method
CalFile

Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
{*
I
Position
InjVol
44
5.0
v+u
3
nana'lO
Positive
8/">
Level
Sample Wt
0.000
')ii"r^
Sequence--MATRIX_pos. sld [Open]
"Sample Name: Matrix
f-
-ment:
Study:
Client:
Laboratory:
Company:
Phone:

Unknown
MATRIXll
Samole lD
Path
01
U(cali bu AData\EDTA\BreweAMAT-Positive
Proc Method
lnst Methocl
Cal File
C:\Xcalibur\methods\EDTA Pos Swabs

Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Position
lnjVol
5.0
Sample Wt
Level
0.000
Sample Name: Matrix 2

Study:
Comment:
Client:
Laboratory:
Company:
Phone:

Unknown
MATRIXl2
Sample lD
Path
02
:U(calibur\Data\EDTA\BreweAMAT Positive
Proc Method
lnst Method

Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
CalFile
Position
InjVol
5.0
6('tq,,\
(zstl
Level
jSample Wt
0.000
{o&
r-l'u
\r
:U(calibu A...\MAT-Positive\Matrix0
-.--
Matrix 6 ("50 ppm")
RT: 0.95
S#: 70
100r
4848899
'-1
t-4
( tsx
c ESI Full ms2 293.00@15.00 [ 125.00-315.001
C :D(ca
libur\...\MAT_Positive\Matrix02
RT:
nqa
S#: 68
M: 8018284
02112107
04:16:49
Matsix 7 ("50 ppm")
1 NL: 1.02E0
+ c ESI Full ms2 293.00@15.00 [ 125.00-315.001
[rx02#ri6 RI:0.93 AV:
NL:9.90E5
rdz= 159.5-160.5 F:
+ c ESI Full ms2
293.00@15.001
125.00-3't5.001 MS
Matnxo2
s*
64
AA: 85'1700
rnlz= 246.5'247 .5 Fi
+ c ESI Fullms2
293.00@15.001
125.00-315.001 MS
Matrix02
8
6
E
o
o
6
&,/
(
1E,-t
:\)(calibur\...\MAT_Positive\Matrix03
OU1Z07 04:27:39
Matrix 8 ('50 ppm')
I NL: 6.61E5
: + c ESI Full msz 293.00@15.00 [ 125.00-315.00]
tafixuitttro Kt: u.gu AV:
RT: 0.90
s#: oo
1001
NL:5.72E5
rn/z= 159.5-160.5 F:
+ c ESI Fullms2
293.00@15.00 I
125.00-315.001 MS
"5-1
Matrix03
5.83E4
ntlz= 246.1247.5 F:
+ c ESI Full ms2
293.00@15.00 [
125.00-315.001 MS
Matrixo3
{r",/+,'
1;'r")
0211?/07 04:38:28
C:U&alibur\...\MAT Positive\Matrix04
RT: nm
S#: oo
1
NL:4.02E5
nVz= 159.$'160.5 F:
+ c ESI Full msz
293.00@15.00 [
125.00-315.001 MS
Matrixo4
AA:
001
"..1
: 5.49E4
rrlz=246.5247.5F:
S#:69
t*-r
+ c ESI Full msz

293.00@15.00 [
125.0G.315.001 MS
Matrixo4
AA:,267123
*l
o"-l
*l
90-.1
*l
MJ
.
c-1
I
70--{
fl
--l
^J
KI:O.ZY
S#:460
M:15177
'NL: 5.07E5
TIC MS Matdxo4
fo +'/,,
(tr\
Matrix 9
f50 ppm')
+ c ESI Full ms2 293.00@15.00 [ 125.00-315.001
C:U(calibuA...\MAT Positive\Matrix05
. Y.YY i
RT: 0.87
S#:64
'*t
ou-i
Matrix 10 ("50 ppm")
02112107 04:49:22
trix05#69 RT:0.94
NL: '1.27E6
Fi
293.00@15.00 [
125.00-315.00t Ms
iilatrixo5
o
o
6
t
o
-=
d
1.62E6
TIC MS Matrixos
2
m
18
16
14
f* rt,t
1iq.r)
NL:1.14E6
+ c ESI Full ms2 293.00@15.00 [ 125.00-315.00]
rVz= 159.$160.5 F:
+ c ESI Full ms2
293.00@15.00 [
125.00-315.001 MS
Metrixos
nlz:- 246.$247 .5
+ c ESI Full ms2
AV:1
.Tb
0211A07 05:00:13
:U(calibuA...\MAT-Positive\Matrix06
NL:1.00E5
RT:
100-l
+ c ESI Full ms2 293.00@15.00 [ 125.00-315.00]
n/z= 159.5-160.5 F:
S*:
+ c ESI Full ms2

293.00@15.00 [
AA:
125.00-31s.001 MS
Malrix06
"u_l
NL:1.16E4
nlz= 246.t247.5 F:
+ c ESI Full ms2
293.00@15.00 [
125.00-315.001 MS
Matrix06
S#;59
10(
A*.52207
9I
u:
8(
71
7(
o
o
G
S#:403
RT: 2.1
M:4747
S#:155
AA:3592
NL:3.25E5
TIC MS Matdx06
6" ++
( tqt
50 ppm EDTA
T}E
C :U(calibu
4...\MAT_Positive\Matrix07
0412107 05:11:03
NL: 1.06E5
RT:0.86
S#:63
AA:5F0515
+ c ESI Full ms2 293.00@15.00
n/z= 159.S160.5 F:
+ c ESI Full ms2
293.00@15.00 [
125.00-315.001 MS
Matrix0T
S#:61
AA:37298
{,
o
G
oJ
o
d
o
RT: 1.42
tno
zo
at Eo
NL:2.63E5
TIG MS MatrixoT
{o t+ro
(ztl
50 ppm EDTA
TTB
OA12l07 05:21:54
:Xcalibu 4...\MAT_Positive\Matrix08
[rix08#63 RT:0.E5 AV: 1 NL: 1.78E5

+ cESl Full ms2 293.00@15.00 [ 125.00-315.001
tu,
RT: 0.85
NL:1.41E5
s#: 63
rn/z= 159.5-160.5 F:
+ c ESI Full ms2
293.00@'15.00 |
12s.00.315.001 MS
AA: 615572
Matrix06
S#:63
E21E3
246.*247 .5 F:
rnlz.--
M:3520'l
+ c ESI Full ms2

293.00@15.00 [
125.00-31s.001 MS
Matrix0E
o
o
RT:5.37
S#: 393
AA:914
g6
f
4
RT: 6.23
S#:456
M:7024
o
6
o
RT:4.12
s*
302
M:3219
RT: 3.37
#:247
M:1382
Kt:o.oz
S#:484
1398
:3.01E5
TIC MS Matrixoo
fv- qq
f /-al <
50 ppm EDTA
'f)P
C :U(calib
ur\...\MAT_Positive\Matrix09
RT:0.83
S#:61
M:
0211?/07 05:32:46
il[uvrcz
NL: 2.08E5
293.00@15.00 [
125.00-31s.001 Ms
Matrixog
10(
8C
T'
7A
oc
o
o
o
-g
x.
TIC MS Matrixog
4.61
11
f x+4b
r3r 6)
6t; u.o+ Av: I
NL: z./cEc
+ c ESI Full ms2 293.00@15.00 125.00-315.00]

[
n/z= 159.S160.5 F:
+ c ESI Fullms2
945379
50 ppm EDTA
C:U(calibuA...\MAT_Positive\Matrixl 0
RT: 0.64
st oz
00-l
'a
AA: 707733
0?/12107 05:43:37
NL:1.54E5
rnlz= 159.$160.5 F:
+ c ESI Full ms2
293.00@15.00 [
12s.00-315.00t Ms
Matrixl0
[-'r +a u
( zl)
50 ppm EDTA
rtnxl0#64 RT: o.EZ AV:
NL: 6.69E4
+ c ESI Full ms2 293.00@15.00

[ 125.00-315.00]
:Xcalibur\...\MAT_Positive\Matrixl
0412107 05:54:29
RT:0.87
S#:64
NL:1.21E0
"r_J
Matrixl
S#:64
1001
: + c ESI Full ms2 293.00@15.00 [ 125.00-31S.00]
n/z= 1 59.5-160.5 F:
+ c ESI Full ms2
293.00@15.00 [
125.00-315.001 MS
1oo] AA:
ftlz= 246.5-247 .5 F:
+ c ESI Full ms2
293.00@15.00 [
125.00-315.001 MS
AA:826545
orl
--l
*-l
Matrixl
'-{
ro-l
rrl
r0-1
el
.s-]
o
o
G
J
o
o
o
RT: 8.51
S#:622
AA:29179
NL:1.48E0
TIC MS Matrixll
10095-
908580-
tv
ol
ou555045-
40-
3F
& uqu
( zqt)
Matrix 1 ('500 ppm')
C:U(calibur\...\MAT_Positive\Matrix 1 2
02fi2107 06:05:20
RT: no5
s#: 70
1001
".J
AA:
293.00@15.00 I
125.00-315.001 MS
Metrixl2
t+ v+t"
(tqo
Matrix 2 ('500 ppm')
C :U(calibu
4...\MAT_Positive\Matrix'l
RT: 0.92
S#:
1001
M:
0412107 06:16:12
n/z=
59.5-1
+ c ESI Full ms2 293.00@15.00 [ 125.00-315.001
60.5 F:
+ c ESI Full ms2

293.00@1s.00 [
125.00-315.001 MS
Matrix'13
nr-l
nJz:246.$247.5F
1
ool
nu-]
AA:
c ESI Full ms2

293.00@15.o0 [
+
125.00-315.001 MS
Matdxl3
"-l
8A
s0-l
7s-1
to-]
"
r:-l
o
o
-l
6
E
o
o
6
TIC MS Matrixl3
ft 4(
(4*
:VcalibuA...\MAT_Positive\Matrix
0?J12107 06:27:03
RT: 0.98
S#: 73
AA:
Matrix 4 ("500 ppm')
F: + c ESI Full ms2 293.00@15.00 [ 125.00-3i5.00]
:2.60E6
TIC MS Matrixl4
libur\...\MAT_Positive\Matrix 1 5
C :D(ca
RT:
stA
161
I
--.1
02112107 06:37:53
NL: 1.87E0
rn/z= 159.&160.5 F:
+ c ESI Full ms2
293.00@15.00 [
125.00-315.001 MS
Matrixl5
fflz= 246.*247.5 F:
+ c ESI Full ms2
293.00@15.00 [
125.00-315.001 MS
MaHx15
o
o
6
!
!
o
o
":
o
E
:2-38E6
TIC MS Matrixls
t,r,t
(4ot

c ESI Full ms2 293.00@15.00 [ 125.00-315.001
<rry
:U(cali bu r\...\MAT_Positivewatrix20
0U12107 07:32:04
500 ppm EDTA

1
RT: 0.86
NL:1.16E6
s#: 63
r/z= 159.s'160.5
F:
AA:
+ c ESI Full ms2

293.00@15.00 [
125.00-315.001 MS
Matdx2O
S#:65
n{z= 246.5-247 .5 F:
F: + c ESI Full ms2 293.00@15.00 [ 125.00-315.00]
'|.03E5
100r
^-l
*l
AA: E38410
.t
+ c ESI Full ms2

2e3.00@15.00 [
125.00-315.001 MS
Matrix20
90-l
I
ru-l
rol
tu-l
'l
'u-]
o
o
{,
d
(-{
(,/',
C:U(calibuA...\MAT_Positive\Matrixl 9
KI: 0.87
NL:1.26E6
S#: 64
1001
AA:
-..1
0?/12t07 07'.21;14
m/=
159.5-160.5 F:
+ c ESI Full ms2

293.00@15.00 [
125.00-31s.001 Ms
Matrixl9
S#:65
t*-] M:71A262
'l
$lr- 246.5-247.5 F:
+ c ESI Full ms2
293.00@15.00 I
12s.00-315.001 MS
Matrixl9
s0-l
'l
80-]
tul
70-..1
*-l
I
. <AEA
S#: 64
AA: 8501922
TIC MS Matixlg
500 ppm EDTA
Tbf
C:WcalibuA...\MAT_Positive\Matrix
RT:0.91
S#:67
100-
"..]
AA:
NL:8.75E5
m/z: 159.$160.5
MatrirlT
1001
,5-l
s0J
es-l
eo]
tr-]
r*l
I
"l
.2 +:r]
&
F:
+ c ESI Full msz

293.00@15.00 [
125.00-315.001 MS
40-l
*l
".-l
30-1
I
25-.],
I
201
I
15-1
1o-l
100-l
*l
'l*1
,l
'l
70J
^-l
o'-l
uo-l
*l
*l
qn-l
ol
oo-1
*l
t,
,tuu
[+o;
+ c ESI Fuil ms2 293.00@15.00

[ 125.00-315.001
C:\)(calibuA...\MAT_Positive\Matrix 1 6
02112107
06:48:38
mx16#6E
1001
RT: 0.89
S#: oo
AA:
Matixl6
s#: ob
*l
"J
159.$160.5 F:
+ c ESI Full ms2
2s3.00@15.00 |
125.00.315.001 MS
^c-l
100:
NL:9.04E5
rVF
AA: 592143
nlz= 246.1247.5 Fl
r c ESI Full ms2
293.00@15.00 [
125.0G.315.001 MS
Malrixl6
sGl
nil
*l
80J
/ c-1
-^l
tu1
--l
fv tl4
( q,"
500 ppm EDTA
RT:0.92 AV: 1 NL:4.32E5
+ c ESI Full ms2 293.00@1s.00 [ 125.00-315.001
{ilF
C:\i(calibuA...\MAT Positive\Matrixl 8
RT: 0.85
S#:
M:
100r
.-l
02112107 07:-10.'21
NL:1.2986
m/z= 159.5-160.5 F:
+ c ESI Full ms2
293.00@15.00 [
125.00-315.001 MS
MetrixlE
:1.57E5
ftlF246.5-247.5 F:
100-
*l
o.-l
9H
c ESI Full ms2

293.00@15.00 [
125.00-315.001 MS
MatrixlS
8J
"-]
ru-l
?0-J
ul
1.61E6
TIC MS MatrixlS
[*q
,
(
\|
4 "t)1
500 ppm EDTA
F: + c ESI Full ms2 293.00@15.00 [ 125.00-315.00]
Seq uence--MATRIX_neg. sld [Open]
Study:
Client:
Laboratory:
Company:
Phone:
Sample Type File Narne

Unknown
MATRIXOl
Sample lD
Path
Proc Method
lnst Method
C
:Xcalibur\Data\EDTA\BreweAMAT_Negative
Cal File
:U(cal ibur\methods\EDTA_N eg_Swabs
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Position
InjVol
5.0
Level
Sample Wt
0.000
******************
Sample Name: Matrix
Study:
Comment:
Client:
Laboratory:
Company:
Phone:
Samole lD
Path
Unknown
MATRIXO2
02
C:Xcalibu AData\EDTA\BreweAMAT_Negative
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
********t***********
.<"I
,lpl-l
,
(
q+b
+"',
paqe
Seq uence---MATRtX_neg. std

[Open]
C- -rnent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
********i********t***ttr******tr***t*tt*****t************t*****a***t**i**************************r***********r**#******r********t*****
Sample Name:
ix 9 ("50 ppm")
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample
Unknown
U+
MATRIXO4
lD
Inst Method
lPath
r./
\Acat t0ur\uata\ts D t RtBrewer\MAT_Negative
Proc Method
rrsg_owaus
Sample Vol
ISTD Amt
DilFactor
0.000
rJ.000
1.000
uar rile
PosIton
InjVol
5.0
Level
Sample Wt
0.000
****************************************ft*t*********t**************s*******t***t**********fi******
T"q
"
6o ,/,/u
( +"r)
lr:
l;l
Seq uence---MATRIX_neg.
Sample Name
sld [Open]
10 ("50
nent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
05
MATRIXO5
Inst Method
:U(calibu AData\E DTA\BrewEnMAT-NEqative
Proc Method
CalFile
u : \xcaltbu r\methods\EDTA_Neg_Swabs
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
Position
10
nJvol
Level
Sample Wt
5.0
0.000
****it******************ts********i******l***********************************r******s**********

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
06
u:
MATRIXO6
Inst Method
xcat
ibu
Proc Method
r\Data\EDTA\Brewer\MAT_Negative
Cal File
C:U(calibur\methods\EDTA_Neg_SweG
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
Posrtron
InjVol
12
5.0
Level
Sample Wt
0.000
**********t********t************#******t************************t*t*******************t*****************i
T,1,,''
t,t
+,/("
/'./4,,,\
Seq uence---MATR|X_neg. sld [Open]

C-'-'ment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Unknown
06
MATRIXOT
Inst Method
U
Path
V(calibu r\Data\EDTA\BreweAMAT_Negatlve
Proc Method
CalFile
\Xcal tbu r\methods\EDTA_N eg_Swabs
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Position
InjVol
12
5.0
Level
Sample Wt
0.000
***********t******************t*****r*******t******tt*t**tt****l*t*****i*****t**+********S*t*****************
Sample Name: 50 ppm

Comment:
Study:
Client:
Laboratory:
Company:
Phone:

Unknown
Sample lD
MAIRIXOE i06
Inst Method
G:
Path
C
:U(calibur\Data\EDTA\BrewenUAt_Negative
Proc Method
CalFile
Position
T'-
U(cal i bu r\methods\E DTA_Neg_Swabs
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
lnjVol
Level
Sample Wt
b.u
0.000
*********t******t***********|****************s**1i
3F
r !1zl't
[+ 4(b
/ ,/,,\/
paqe 4
Sequence--MATRIX_neg. sld [Open]

l^ .ment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample Type
Unknown
ile Name
MATRIXO9
Sample lD
Path
06
Inst Method
G
xcali
bu
\Xcalibu r\Data\EDTA\Brewer\MAT_Negative
Proc Method
CalFile
r\methods\E DTA_Neg_Swabs
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
Position
InjVol
12
5.0
Level
lSample Wt
0.000
*t*********t************************************************t***********i****i*******i********t*t********

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
12
MATRIXlO
Inst Method
C :U(cal
:U(cal ibur\Data\EDTA\Brewer\MAT_Negative
Proc Method Cal
File
Position
ibur\methods\EDTA_Neg_Swabs
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
InjVol
112
Level
Samole Wt
5.0
f"i]
{r q(b
(
+,4
page 5
+lel"'r
Seq uence---MATRIX_neg. sld

[Open]
rent:
Study:
Client:
Laboratory:
Company:
Phone:
Unknown
MATRIXI
Sample lD
Path
01
u:
Inst Method
\ cailDu r\uata\tsDTA\Brewer\MAT_Negative
Proc Method
C:U(calibur\methoW
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
Cal File
Position
InJvol
5.0
Level
Sample Wt
U.UUO
tt*******t******t**i*********t**************************t******************t***********t**************ft**#**************r*******ffi******
Sample Name: Matrix
ppm")
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
02
C:U(calibu r\Data\E DTA\B rewer\MAT_N egative
MATRIX12
Inst Method
Proc Method
Cal File
L;:\Xcattbur\methods\EDTA_Neg_swabs
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
Position
InjVol
5.0
Level
Sample Wt
0.000
****s*******************t**t***t*****i*************t**$*********i****************fr*************f**********
doF
vltzl
v4b
('l,l)
naoe 6
o1
Seq uence---MATR tX_neg. std

[Open]
Sample Name:
.'nent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
**********i****************t***tt****t*****i**i**********************1***t******t**t***********************friit******t***r***t*********r
Sample Name: Matrix
ppm")
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
MATRIXl4
04
U: \Xcati
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
bur\Data\EDTA\Brewer\MAT_Negative
*******t**********************t******t*************************i***K****r*****
*****************************
5"P
> lrr
C qqb
( +,+)
l"]
Sequence---MATRtX_neg. sld [OpenJ

/
Sample Name:
C- .ment:
Study:
Client:
Laboratory:
Company:
Phone:
sample Type File Name
Samole lD
Path
Unknown
MATRIXl5
06
u:\
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
canDur\lJata\EDTA\Brewer\MAT-Negative
********t***************i*****t*t*************st**t******t***********ra************tr***

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.tJ00
************i***ft**********************s****i*t**t*******i**i****t*r********
***t***************tr******i*#
5rP
')
[+
rLAb
(+,)
lfl"1
Seq uence---MATR lX_neg. sld

[OpenJ
Sample Name:
ppm EDTA
C--.ment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.u00
ffi*iff#s******#****lt*********i***ft*t*********a************t*ffi****t********t***********
Sample Name:
ppm EDT,
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
MATRIXlS
06
u ; \AcatrDu r\uala\tsD
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
Rtgrewer\MAT_Negative
*******il*******************+****t******i************i********i********t****************t****************H*****************s**t********
.PP
r,
z,\
+Ale
\
Iq/b\
'./
ttl "1
Seq uence--MATRIX_neg. sld [Open]

Sample Name:
ppm EDTA
C^-ment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
06
MATRIX19
Inst Method
Xcalibu r\Data\EDTA\Brewer\MAT_Negative
Proc Method
CalFile

Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
Position
InjVol
11
5.0
Level
Sample Wt
0.000

Comment:
Study:
Client:
Laboratory:
Gompany:
Phone:
Sample lD
Path
Unknown
06
C:U(cal i bur\Data\EDTA\Brewer\MAT-N egative
MATRIX2O
Inst Method
Proc Method

Sample Vol
ISTD Amt
DilFactor
0.000
0.0u0
1.000
CalFile
Position
InjVol
11
5.0
Level
0.000
********************t*
*?
'r l1r
tL TUc
'r)
/+,
',/
lSample Wt
l:1
:I(calibuA...\MAT_Negative\Matrix0
02113107 09:05r10
RT:0.92
NL:2.75E4
MA:
Matrix 6 ('50 ppm')

RT:1.04
AA:493664
nlz= 272.5-273.5F: - c
ESI SRM ms2

291.20@15.00 I
NL: 2.93E4
rvz= 299.5-300.5 F: - c
ESI SRM ms2

344.20@15.00 I
246.fi-247,50.'
272.50-273.50i MS
Matrix0l
100
299.50-300.50.'
325.s0-326.50t MS
Matnx0l
AA:9539
I
7
RT:5.98
AA:6699
70
.:o
.g
M:13.09
rnlz=282.8-2t43 F: - c
ESI SRM ms2
133?39#;'3't"'
Matrixol
f*++t
Time (min)
:4.61E3
m/z= 3l1.$312.5 F: . c
ESI SRM ms2
356.00@15.00 l
1.50-312.501-Ms
Matrix0l
31
:Xcali
buA...\MAT_Negative!Q[i51Ql
2.2 o ^'r
0Afi107 09:05:10
RT:0.92
MA:164222
NL: 2.75E4
rnlF 272.1273.5 F: - c
ESI SRM
ms2
291.20@1s.00 t
246.50-247.50.'
272.50-273.s01 Ms
Marix0l
AA:9539
1001
nu-l
roJ
85J
8o-l
'5J
to-1
RT:1.00
AA:6396
65--l
^.]
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d
0
o
RT:4.79
M:24421
rlF
282.8-2U.3 F: - c
ESI SRM ms2
30320@15.00 r
282.75-2U.2g''MS
Matrix0l
nVz= 311.9312.5 F: - c
ESI SRM mu
356.00@15.001
311.s0.312.501 MS
Malrix0l
(4q
(u,')
:\)(calibuA...\MAT_Negative\Matrix02
02/13107 09:16:25
Matrix 7 ('50 ppm")
XI: n9t
t@r
MA: 71145
RT:1.12
AA:404878
m/z= 299.$300.5 F: - c
ESI SRM ms2
344.20@15.00 I
299.50-300.50.'
325.50-326.501 MS
Matnx02
"J
RT:5.02
AA:24793
RT:8.54
AA:25064
NL:2.42E4
tr z= 325.t326.5 F: - c
ESI SRM ms2
li833gJ333r
RT:0.93
P
pG
I
o
o
RT: 7.47
AA: 28157
4.1083
trVz= 31 1.5-312.5 F: - c
ESI SRM ms2
356.00@15.00l
311.50-312.501 MS
Matnx02
{auva
C:\Xcalibur\...\MAT_Negative\MatrixO2
Zu
rA
0413107 09:16:25
t'lz= 272.1273.5F: -
RT: 1.12
NL: 2.75E4
AA:404878
ESI SRM ms2
rtz= 299.5-300.5 Fi - c
ESI SRM ms2

344.20@1s.00 I
299.50-300.50.-
3il33.9ii33,r
272.50-273.501 MS
Matrix02
tzs.so-gze.soi t,ts
Matrix02
RT:0.85
MA: 71145
RT:5.02
AA:24793
RT: 8.54
AA:25064
x
o
J
o
o
NL: 4.1 0E3

nl/z= 31 1.5-312.5 F: - c
ESI SRM ms2
356.00@15.00 [
311.50-312.50t MS
Matrix02
f+aab
(va)
:lKcalibur\...\MAT_Negative\Matrix03
02113107 09:27:20
RT:1.08
MA:45079
NL:6.55E3
(1,6
RT: '1.11
NL:2.1184
M:yl440
rnlz= 272.5-273.5 F: . c
ESI SRM ms2
291.20@15.00 [
299.5-300.5 F: - c
ESI SRM ms2
344.20@15.001
299.50.300.50.rTYz=
246.fi-247.50.
272.50-273.501 MS
325.s0-326.50j MS
Matix03
Matrix03
RT:4.79
AA:23007
M:722U
RT:1.08
MA:
rnlz= 246.U247 .5 F: - c
ESI SRM ms2
291.20@15.00 t
246.&-247.sO.272.s0.273.50i MS
Matrixo3
RT: 6.24
M:5927
RT: 4.67
AA:'15672
10h
ss-l
I
eoj
M:70?4
ttlz= 282 .8-294 .3 F i - c

ESI SRM ms2
303.20@1s.oo I
282.7r2U.251 MS
Matrixo3
^-l
-'t
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8o-J
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m/z= 31 1.5.312.5 F: - c
ESI SRM ms2
3s6.00@15.00
311.50-312.501 MS
Matrir03
:U(calibur\...\MAT_Negative\Matrix04
02113107
g-fggr)
09:38;15
NL: 3.72E3
rtlz=272.5-273.5F: - c
ESI SRM ms2

291.20@15.00 I
246.50-247.50.'
272.s0-273.50i MS
Matfix04
RT:0.93
M:'18721
RT:8.43
AA:10471
RT:4.33
AA:49753
RT:6.78
AA:33233
RT: 8.32
^d'|22537
RT:5.02
AA:13436
mlz=246.5-247.5 F: - c
AA:80921
ESI SRM m2
291.20@15.00 t
246.50-247.50.-
272.50-273.50i MS
Matrix(X
o
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M:,4324
? t7tre
1001
Yl
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C:\Xca libur\...\MAT_Negative\Matrix05
10q
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02113107 09:49:09
NL:3.45E3
n/z=272.5-273.5 F:. c
NL: 1.66E4
ESI SRM ms2
rvz= 299.5-300.5 F
ESI SRM ms2
lit?8.@;i.Ht
i33:38ffi3r
272.50-273.s01 Ms
Matrix05
325.50-326.501 MS
Matdx0S
@
o
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:3.19E3
m.tz= 282.E-284.3 F'.
ESI SRM ms2

303.20@15.00 I
.c
282.7$284.251-MS
Matdx05
: 4.35E3
rVz= 3'l 1.$312.5 F; - c
ESI SRM ms2
356.00@15.00 I
311.50-312.50t Ms
Matnx0S
{o4
(
4t*\
:l(calib ur\...\MAT_Negative\Matrix05
rol
RT:1.15
RT:0.85 AA: 17456

AA:'170i 9l
-l
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02113107 09:49:09
'Matrix
10 ("50 ppm.)
\),0
NL:3.4583
rr'Jz=
NL: 1.68E4
272.5-273.5 F: . c
ESI SRM ms2

291.20@1a
!_5.99 t
ffz= 299.5300.5 F: - c
ESI SRM ms2
246.50-247.50.
246.50-247
272.50-273.501 Ms
ti3 339J3 33 r
Matnx0S
325.50-326.50t Ms
Matrix0S
10(
MA:16635
2.71E3
rVF 325.5-326.5 F:
9l
ESI SRM ms2
344.20@15.001
299.50-300.so.-
ar
szs.so-sze.soi
MatrixoS
-c
ts
8C
75
70
9.0
o
o
o
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-q
1{L:8.44E2
nlz= 282.8-28/.3 F: - c
ESI SRM ms2
13!:?&_9lf39t",
{e
+vr,
/s,
m/z= 3'1 1.$312.5 F: . c

ESI SRM ms2
356.00@15.00 I
311.50-312.501 MS
Matrix05
:U(calibur\...\MAT_Negative\Matrix06
NL:5.45E4
rvz= 299.5-300.5
ESI SRM ms2
344.20@15.00 |
F:
299.50-300.50.325.50-326.50i Ms
Matrixo6
-NL:
1001
6.39E3
m/z:2465247.5 F: - c
,5-l
371'*;g1fH.l
'oJ
r5-j
272.5G273.501 Ms
Matrix06
eo-..1
'J
I
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oc-l
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"""-]
ESI SRM ms2
331?l_gJfi3lr",
{o
qq'
t^)
.c
:\XcalibuA...\MAT_Negative\Matrix07
02113107 10:10:S4
50 ppm EDTA
RT:0.78
r00-l
*l
q<-l
AA:
rnlz= 272.5-273.5 F: - c
rvz: 299.$300.5
ESI SRM ms2
1s.00 [
F: - c
ESI SRM ms2
3?l:3391i33
272.50.273.501 Ms
272.50.273.sol
It3339J333r
MatdxoT
325.50-326.501 MS
MatrixoT
NL:2.69E4
rnlz= 246 .*247 .5
ESI SRM ms2
291.20@'15.00 |
:-
rvz= 325.5-326.5 F: - c
ESI SRM msz
3ZtZ391iH.r
6
272.50-273.sot Ms
t63339J333r
Matrix0T
325.50-326.50t MS
MatnxoT
I
7
70
oo
o
J
o
a
o
10G1
^-l
'"-l
--l
1 ftjlz=282.8-2A43F:-c
miz= 3'11.5-3'12.5 F: . c
ESI SRM ms2
356.00@15.00 l
311.50.312.501 MS
Malrix0T
ESI SRM ms2
30320@15.00 [
282.79284.251-MS
Matix0T
ru-J
r-l
trl
to-]
*l
ro-l
*l
s-l
*l
45-.{
,^l
t:l
"l
'-t
?NJ
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(*r)
:\Xcalib u r\...\MAT_Negative\Matrix08
RT: o.78
r09
AA:
02113107 10:21:43
NL:5.8885
rr/z= 272.1273.5F: - c
50 ppm EDTA
RT: 0.81
AA:
ESI SRM ms2

29120@'t5
r5.00 I
246.50-247.50.'
246.50-247
NL: 2.34E4
r/z= 299.$300.5 F: - c
ESI SRM ms2
!333&J333r
272.50-273.s0t Ms
325.50-326.50i MS
Matrix0S
Matrix0S
RT:8.55
AA:23320
RT:5.41
M:15034
ffilz=246.1247,5F: - c
RT: 1.35
ESI SRM ms2
72]6.391 :3.r
272.50-273.50t Ms
MakixoS
o
f
e
o
a
o
n/z= 311.5-312.5 F; . c
ESI SRM ms2
3s6.00@15.00 [
311.50-312.501 MS
MatrixoS
6e
+*.
1+at)
:\j(calibuA...\MAT_Negative\Matrix09
-
0?/13107 10:32;34
RT: 0.78
1001
50 ppm EDTA
tu
NL:4.27E5
M:
RT: 0.81
rnlz= 272.5273.5 F:. c

ESI SRM msz
291.20@15.00 r
ss-l
AA:
246.s0.247.s0.'
zzz.so.zzg.soi
rxp
NL: 7.48E3
m/z= 299.5-300.5 F: - c
ESI SRM ms2
3/t4.20@15,00 t
299.50-300.50,325.50-326.501 MS
rr,rs
Matrix09
Matrix09
: 5.48E3
100
rYz= 325.5-326.5 F:. c
ESI SRM ms2
344.20@15.00 [
299.50-300.50.325.50-326.501 MS
Matrixo9
90
6
80
RT:2.12
Ai\:17290
o
I
6
a
.E
RT:0.89
M:7072
RT:8.20
AA:23505
filz= 282.6-2U.3 F:. c
NL: '1.68E3
282.75-2U.251 MS
ESI SRM ms2

s56.00@15.00 [
311.50-312.50t MS
Matrix09
ESI SRM ms2

303.20@15.00
1s.00 II
rvz=
31
1.5-3'12.5 F: - c
:\lXcalibur\...\MAT_Negative\Matrix
RT:
M:
02113107 10:43:28
50 ppm EDTA
NL:2.64E5
nlz=272,5-273.5F: - c
ESI SRM ms2

291.20@15.00 I
246.50-247.50.'
272.50-273.50i MS
Matrix'|0
1001
rilz= 325.5-325.5
nl
F: -
ESI SRM ms2

344.20@15.00 t
299.50.300.50.-
'l
'l
ses.so-sze.soi l"ts
Matrixl0
ro1
7l
7o-]
os]
o
tr
6
!
.:o
G
NL:4.87E3
1ocr
r/z=
'"J
31 1.5-312.5 F:. c
ESI SRM ms2
3s6.00@15.00 l
"-J
Matrix'10
311.5G312.50t'MS
'l
ro-l
'-l
zo-]
*-l
uo-1
*l
*-l
,u-l
40J
^-l
Jl
.o-]
{^t
Hu
(+t)
rol
fiYz= 325.$.326.5 F: - c
ESI SRM ms2
344.20@15.00 I
95-.{
*.]
299.50-300.50,
325.50-326.501 MS
Matrixl l
85-l
rol
;:l
os-]
o ^^l
9",-]
00-
^-l
*l
ESI SRM ms2

356.00@15.00 [
311,50-312.501 MS
Matrixl l
e0-1
--l
^-l
80-l
I
,R)
70-J
^-l
o"-l
^^l
o"l
*l
*t
4s-l
40-l
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--l
^^l
"u-l
{*qt
:XcalibuA...\MAT_Negative\Matrix
1001
*l
RT: 0.
MA: 1
0Z13lO7 11:05:13
nx(,
NL: 8.32E4
299.5-300.5 F: . c
ESI SRM ms2
344.20@15.00 I
299.50-300.50.
325.50-326.501 MS
'n,lz=272.*273.5F: -c
r/z=
ESI SRM ms2

291.20@15
r5.00 [
246.50-247.fi,
246.50-247
272.50-273.50t MS
Matrixl2
Matrixl2
nl/z= 246.$.247.5 F: - c
ESI SRM ms2
291.20@15.00 I
246.50.247.50.
272.50.273.501 MS
Matdxl2
o
3
4.1
7E3
.t312.5 F: . c
ESI SRM ms2
356.00@15.00 [
3't '1.50-312.501 MS
nvz:
311
Matrix 12
fouqa
C:U(calibur\...\MAT_Negative\Matrixl 3
rol
'l
*-J
'l
0?/13107 11:16:02
qlp
tnlz=246.5-247.5 F: - c
ESI SRM ms2
291.20@1s.00 [
246.50-247.fi.
272.s0-223.50i Ms
Matnxl3
'l
1.1
701
.'-]
^*l
rf'lz= 262.&1943 F: - c
ESI SRM ms2
rvz=
31
282.7*28{251 MS
Matrix'13
356.00@1s.00 I
311.50-312.501 MS
Matrixl3
fl,t'tt,
(4
1.5-312.5 F: - c
ESI SRM ms2
30320@15.00 I
3)
C :U(calibu
r\...\MAT_Negative\Matrix 1 4
02J13107 11'.26:52
RT:1.15
100r
MA:2097890
,'-1
rnlz= 272.12735F: - c
ESI SRM ms2
291.20@15.00 [
246.50.247.50.
272.5S273.501 MS

RT: 1.27
NL:3.67E4
AA:1194082
rnlz= 299.$300.5 F: - c
ESI SRM ms2
344.20@15.00 [
299.50-300.50,
325.50-326.50t MS
Matrix'14
Matrix'14
RT:4.25
M:24620
RT:6.78
RT:7.78
AA:27941
16
: 1.49E4
RT: '1.'15
.E
RT:3.18
AA:1E839
NL: 5.02E3
nlz= 242.8-2U3 F: - c
rvz=
ESI SRM msz

303.20@15.00 I
282.7r2U.251 MS
.t312,5 F: -
311.50-312.50t MS
Matrixl4
Matrixl4
RT: 4.12
M:10676
fuqte,
31
ESI SRM ms2

3s6.00@15.00 I
:\jXcalibur\...\MAT_Ne gative\Matrix
02/13n7 f:37:47
<Jhg
NL: 4.94E4
rnlz= 299.5-300.5 F: - c
ESI SRM ms2
344.20@15.00 |
299.50-300.50.325.50-326.501 MS
irlatnx'15
pT.
RT:6.86
AA:54615
?
na
3562
RT: 5.10
AA: 50970
10(
80
RT:0.93
AA:138673
/5
65
RT:3.84
AA: 38576
Io
l
e
o
5o
RT:7.36
AA:24214
RT:6.06
AA: 18141
RT:2.57
RT:6.28
AA:7102
Nz= 282.8-2U.3F: - c
ESI SRM ms2
30320@15.001
282.7$2U.251
MatnxlS
5.
/
MS
q,/U
4'.)
: 1.78E3
:Xcalibur\...\MAT_Negative\Matrix,t 6
RT:0.8S
.rol*"rt*
'll
02113107 11:48:42
clop
- tu
NL:2.1286
rnle 272.5-273.5 F: - c
RT: 0.89
AA:
ESI SRM ms2
NL: 2.31 E5
rvz= 299.$.300.5 F: - c
ESI SRM ms2
lit?P;i#l
u4.20@15.001
272.50-273.501 MS
299.50-300.50.'
325.50.326.501 MS
MatrixlS
Malix'16
4.38E3
325.5-326.5 F: - c
r/z=
ESI SRM ms2
344.20@15.001
299.50-300.50.'
325.50-326.50t Ms
Matnxl6
o
o
RT: 1.27
M:11820
o
o
o
RT:4,18
AA:4894
ntz= 282.8-28(.3Fl. - c
ESI SRM ms2

303.20@15.00 t
282.7$284.251- MS
Matrixl6
5.qru
(+t)
C:U(calibur\...\MAT_Negative\Matrix I 7
RT:0.85
0213107 11:59:36
NL:2.29E6
AA:
trtz= 272.5-273.5
500 ppm EDTA

RT:
AA:
F: - c
ESI SRM nrs2

291.20@15.00 I
246.s0. ,47.50.'
NL:2.5685
trVz= 299.5-300.5
ESI SRM ms2
F:.
344.20@15.00 I
272.50-273.50t MS
MatrixlT
299.50-300.50.'
325.50-326,501 Ms
Matrix'17
.'].lz= 246.5-247.5
F: - c
ESI SRM ms2
100
AA:29498
3il33g.'i33r
90
i33339J333r
272.50-273.501 MS
MatrixlT
m/z= 325.5-326.5 F: - c
ESI SRM ms2
325.50-326.501 Ms
Matnx'|7
80
RT: 0.86
AA:38925
70
oc
o
!o
RT:1.73
AA:
M:4728
trVz= 31
1.5-312.5 F: .
ESI SRM ms2

356.00@15.00 I
311.50-312.501 Ms
MalixlT
O,t4,/6
io ( qtt\
C :\Xcatib u
.
't001
r\...\MAT_Neoative)gllx,lg_
RT: 0.85
1511
M:
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100
VJ
0?J13107 12:10:25
500 ppm EDTA
tu
AA:926981
RT: 0.89
AA:
fiilT= 272.*273.5 Ft . c
ESI SRM ms2
291.20@15.00 [
ESI SRM msz

344.20@15.001
246.50-247.50.
272.5G273.501 MS
MatrixlE
.':r'z=
299.50-300.50.'
325.50-326.501 MS
MatrixlS
246.1247.5 F: - c
ESI SRM ms2
29120@1s.00 [
246.50-247.50.
zzz.so-zzs.sol
Matflx18
us
80
T'
70
I
6
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{o
sEo
mlz= 282.6284.3 F: - c
ESI SRM ms2
303.20@15.00 [
282.7U2U.251 MS
MatrixlE
ft+,+a
NL:2.3385
rvz= 299.$300.5 F: -
C:U(calibur\...\MAT_Negative\Matrix 1 9
RT: neE
1
00- AA:
ar-l
15f
02113107 12:21:15
500 ppm EDTA
NL: 1.42E6
ffilz= 272.5-273.5 F: - c
ESI SRM ms2
291.20@15.00 [
<l-D6
NL: 2.82E5
m2= 299.5-300.5 F: - c
ESI SRM msz
344.20@15.00 I
246.50-247.50,
?72.s0-273.50t MS
Malrixl9
299.50.300.50.
325.50-326.50i MS
Matrixl9
NL:6.55E4
atz= 245.$247.5
F: -
ESI SRM ms2

291.20@15.00 I
RT:3.72
AA:19293
GDfFlroi-l
-q
RT:4.56
AA:6280
NL:3.99E3
rr'lz= 282.A-2U3F: - c
ESI SRM ms2
303.20@1s.00 [
282.7r2v.25t
Matrixl9
MS
r/z= 311.5-312.5 F: - c
ESI SRM ms2
356.00@15.001
3r'1.50-312.s01 MS
Matnxl
44a
(vtr)
C:l(calibur\...\MAT_Negative\Matrix20
RT: 0.85
AA: 169r
02113107 12:32:06
NL:1.67E6
RT:0.96
ntlr272.5-273.5F: - c
NL:2.18E5
,Qq:
rnlz= 299.5-300.5 F: . c
ESI SRM ms2
r5.00 I
ESI SRM ms2
291.20@15.001
246.50-247.50.'
133339J33,1r
272.50-273.501 MS
Matnx20
325.50-326.50j MS
7.12E3
10(
ol
80
/5
70
o
6
o
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RT: 3.11
AA:'13513
RT: 8.85
t*r
*l
M'J
*l
trYz= 31 '1.5-312.5 F: - c
ESI SRM ms2
355.00@15.00 [
311.50.312.501 MS
Matrir0
8s-J
I
801
--l
,t-.']
RT:5.38
M:6106
70-.i
^-l
^^l
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--l
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40-l
^-l
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Positive lonization Mode- Matrix Effect

EDTA free brood swabs- extracted then spiked
to be 50 ppm EDTA
Area of RIC ior base p""r
tifo'*Ll
Sampte
2
3
1
AVERAGE
33iff3:
4ffi6115
4
5
2840952
12647507
6598351.4
Neat EDTA sotution- S0 ppm
Injection
AVERAGE
Area of RIC for base peak (160 m/z)
1
2
3
4
5
557891
550515
615572
945379
70773g
67s41g
Matrix Effect (50 ppm), %
976.9285687
EDTA free blood swabs- extracted then spiked

to be s00 ppm EDTA
Area of RtC ior base peak (iOOrnlrl
Sample
AVERAGE
1
2
3
4
5
9410131
2$08297
18080488
22902136
1ilfl570
$169724.4
Neat EDTA sotution- 500 ppm

Injection
AVERAGE
Area of RtC for base peak (160 m/z)
1
2
3
4
5
5957879
6957758
6983927
6279487
3687103
7772030.8
233.7062843
{*
+qa
&,a,\
r,( u l.,r
avF
NEGATIVE lonization Mode- Matrix Effect

EDTA free blood swabs- extracted then spiked
to be s0 ppm EDTA
Sum of Areas of free EDTA peaks (mtz 273 + 247)
Sample
1
2
3
4
5
AVERAGE
170618
74496
79143
$721
17019
B7g4s
Neat EDTA sotution- S0 ppm
Injection
Sum of Areas of free EDTA peaks (mtz273 + 247)

1
1206757
1790660
2
3
4605670
3956765
2901483
2892267
AVERAGE
3.040694376
EDTA free blood swabs- extracted then spiked to be

s00 ppm EDTA
Sum of Areas of free EOTA peaks (mlz 273 + 247)
Sample
AVERAGE
1
2
3
4
5
10962262
p608318
569737
2147727
2144609
5766530.6
Neat EDTA solution- 500 ppm

Injection
Sum of Areas of free EDTA peaks (mlz2|3 + 247)
I
14785267
8893392
16049375
16831807
1 7809391
16873846.4
2
3
4
5
AVERAGE
34.1743694
f*
zlllt't
qqn
( vva)
1-pp
SPOT STZE L.O.D.
uuo
6(v+a)
lw
02tr5t2007
Blood spot sizes
(l
uL, 5 uL,
10
uL)
f*
+vb
&+v)
Sequence--Spot Size_pos.sfd
[OpenJ
Study:
Client:
Laboratory:
Company:
Phone:
sample lD
Unknown :Spom-
Path
C : U(ca
li b
r\m
-I
odslEDil-F
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
*****t*******t*t**********t**********
Sample Name: 1uL
t*******************t****t**l*************t*****************************t**********rr
+A
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
lnst Method
'\Xnelihr
Proc Method
CalFile
TA_Pos_Swa
Position
InjVol
5.0
j0.000
I
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
****l********************t**t**************t************************************t**********************************itr
&
uo,
(vv;)
z/rr/"r
Tl?P
Seq
uence--Spot Size_pos. sld

[Open]
Sample Name:
'nent:
Study:
Client:
Laboratory:
Company:
Phone:
:Xcalibur\D@
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
*********************************t************************************i*******t*************************i*********r********r******i*****f*****
Sample Name:1
Comment:
t-l
Study:
Ctient:
Laboratory:
Company:
phone:
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
**t***************************************************s****************t*******************************i*****i*tr**********************tr*****
f,
(
urc
v+)
>ltr ["r
ttr{]
Sequence--Spot Size_pos. sld

[Open]
Sample Name:
C- -menf
Study:
Client:
Laboratory:
Company:
Phone:
lnst Method
Proc Method CalFile

tEUtuus\EU
lA _f,os_Swabs
Position
InjVol
53-
Level
Sample Wt
0.000
***********************************************************t***t***************************t*****************t***************f***************
Sample Name:
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample TypG File Name
Sample lD
Unknown
04
Spot06
lnst Method
\Xcalihr
Path
:u. u\cat
our\uata\ts D I A\Brewer\s pot s ize_positive
Proc Method CalFile
rr\rnath;;.\trnr^
sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Position
lnjVol
5.0
Level
Sample Wt
0.000
*******t***********i******ft****H*t*****************************************************t*****************tr***********r*********i************
foq&
kvt)
lgl"t
s,)p
Seq uence--Spot Size_pos. sld

[Open]
Sample Name:
C--.rnent:
Study:
Client:
Laboratory:
Company:
Phone:
A\Brewer\Spot Size_posi
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
uL
+A
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Inst Method
Proc Method
'J(caiiburimeiffi
Sample Vol
ISTD
u.000
0.000
Amt
CalFile
Position
hJVol
5.0
Level
ple
Factor
]Dit
1.000
t********t********t*****t***************t**t******************************r*********e*s*
o4-
4k-,
(v q4
zlr
l't
T]1P
Sequence--Spot Size_pos.sld [Open]

Sample Name:
blood swab extract
C^-.ment:
Study:
Client:
Laboratory:
Company:
Phone:
C:U(calibur\De
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
*******************i********************t*******i***t*************************************s******t*************************it************t*
Sample Name:
5ULEDTA+B
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
f"
uu"
(u+r)
zls l,t
5vp
Sequence---Spot Size_pos. sld [Open]

Sample Name: Neg blood swab extract
rtent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
01
Spot11
lnst Method
C :U(cali
:U(cal ibu r\OataE
Proc Method
Otn@
Cal File
bur\metho0G\EDTn pos5vabs
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Position
InjVol
5.0
Level
Sample Wt
0.000
Sample Name: 5 uL EDTA +

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Samole lD
Path
Unknown
07
C:
Spot12
Inst Method
Sample Vol
0.000
\)(cal bur\Data\E DTA\eretedS pof

i
Proc Method
ISTD Amt
10.000
Cal File
ite
positive
Position
InjVol
5.0
Level
Wt
0.000
DilFactor
1.000
C'/ 4fu
(+s")
zlrrl"'t
g)p
Sequence--Spot Size_pos.sld [Open]

Neg blood swab extract
Study:
Client:
Laboratory:
Company:
*******t****************f
Sample
Comment:
****t*************l
****t*********i************
TPF
10 uL EDTA + A
Study:
Client:
Laboratory:
Company:
Phone:
lSample Wt
zlrr("1
8" +tt'
( vs)
5W)
Sequence---Spot Size_pos.sld [Open]

blood swab extract
Sample Name:
C-
Study:
'nent:
Client:
Laboratory:
Company:
Phone:
Sample Name:
Comment:
1O
uL EDTA +
T0fl
Study:
Client:
Laboratory:
Company:
Phone:
*******t********************************t*i*********
***************t****t**
LL q4b
(v:4
>hr
l"t
./tp
Sequence--Spot Size-pos.sld [Open]

Study:
Client:
Laboratory:
Company:
Phone:
*****l**l*************t*****************
**i*i***a*****************t*************i************t***********f*s*****i*****
Sample Name: 1O uL EDTA + C

Comment:
$F
Study:
Client:
Laboratory:
Company:
Phone:
Sample Wt
*******tt**************************************t*******
t* ++a
i\
t''/ 4S)
nana
>
ls 1"1
1p
Sequence--Spot Size-pos. sld [Open]

Sample Name:
swab extract
Study:
C-'-nent:
Client:
Laboratory:
Company:
Phone:
**t*********a******i****t***i*it**********t*********************t****************************
*.
51''? f@
54-rot
9," L wil , (/Nctr { ^C

u"rttt fttCd^4zer-/ ot1eczeV .
s 2;24^/
cG' &TL
lhr
t*
qon
( v'4
vlrrl't
5'rP
C:l(calibur\...\Soot0
0A15107 1'l:46:31
Full ms2 293.00@1 5.00 [ 1 25.001 5.00]

nvz= 159.$160.5
F: + c ESI Full ms2
293.00@15.00 [
125.00-315.001 MS
Spotol
nlz-246.sl47.5
F: + c ESI Full ms2

293.00@15.00 I
125.00-315.001 MS
Spotol
t+-+a
('/t)
151
0?i15107 11i57'.42
NL:2.79E4
nvz= '159.5-'160.5
F: + c ESI Full ms2
293.00@15.00 I
125.00-315.001 MS
Spot02
f* qqo
ftl
+ c ESI Full ms2 293.00@15.00

[125.00-315.001
C:U(calibur\...\SpotO3
02115107 12:08:34
NL:
+ c ESI Full ms2 293.00@15.00

[ 125.00-315.001
r/z=
159.$.160.5
F: + c ESI Full msz
293.00@1s.00 [
125.00-31s.001 Ms
Spoto3
4.08E3
'r],lz=
246.$247.5
F:+cESl Fullms2
293.00@15.00 [
125.00-315.001 MS
Spol03
6:
8C
/a
7C
o
o
oa
o
-g
: z.o/ Ec
TIC MS Spoto3
140
,q
120
1.63
619
EJ6
71
375
5.12
(t{5
(+s)
02115107 12:19:30
NL:2.37E4
rru2= 159.$150.5
F: + c ESI Full ms2
293.00@15.00 I
125.00-315.001 MS
Spot04
rnlz= 246.5-247 .5
F: + c ESI Full msz
293.00@15.00 [
125.00-315.001 MS
Spot04
1001
nu-1
*l
ru-l
ro-J
75-1
I
70-l
--l
--l
o ^^l
l,
"r-l
s97
I ta
r
b3b
f^r 4ao
( ts*)
+ c ESI Full ms2 293,00@15.00 [ 12s.00-315.00]
C:U(calibuA...\SpotO5
02115107 12:30:35
o
o
o6
o
o
6
NL: 2.93E5
TIC MS Spotos
&-,tq,.
(qs>
c ESI Full ms2 293.00@15.00 [12s.00-315.001
C:U(calibuA...\Sooto6
+ c ESI Full ms2 293.00@15.00 [ 125.00-315.001
1001
^-l
"l
onl
::l
"l
ro-]
'l'-t
-:l
2.81
I
225
fadT
fo
uu
C:U(calibur\...\Spot07
02115107 12:52:22
ot07#65 RT:0.89 AV:

NL: O
rn/z= 159.$'160.5
F: + c ESI Full ms2
293.00@15.00 [
125.00-315.001 MS
Spot07
:2.02EJ
1001
*l
90-l
rnlz= 246.*247 .5
F: + c ESI Full msz
293.00@15.00 [
125.00-3'l5.0ol Ms
SpotoT
.J
*l
ro-]
tr-]
70-1
cr-.1
--l
o
o
^"-l
.2
6
o
1.75E5
Tta MS Spoto7
e
k)
NL:4.76E3
+ c ESI Full ms2 293.00@15.00 [ 125.00-315.00]
02115107 01:03:17
C:\)(calibuA...\Soot08
NL:
4.5?E4
n/z= 159.t160.5
'100-l
F: + c ESI Full ms2
^_l
2e3.00@15.00 [
'"-l
125.00-315.001 MS
Spot08
1.39E4
,::
*l
ro-l
*t
n/z= 246.5-247.5
F: + c ESI Full ms2
293.00@1s.00 [
125.00-315.001 MS
Spot08
ro-l
'l.-l
6s-i
o --I
656--NL:2.90Es
8.97
216
TIC MS Sool08
237
3.24
2.95
&++,
(
+ua)
: + c ESI Full ms2 293.00@15.00 [ 125.00-315.00]
:Xcalibur\...\Spot09
02115107
01:14:09
+ c ESI Full!ns2 293.00@15.00 [ 125.00-315.00]
NL:0
rn/z= 159.$160.5
F: + c ESI Full msz
293.00@15.00 [
125.00-31s.001 Ms
Spoto9
6.45E3
rnlz= 246.5-247 .5
F: + c ESI Full ms2
2e3.00@15.00 [
'125,00-315.001 MS
Spot09
o
o
o
E
o
o
TIC MS
SpotO9
&ova
(+,"t)
02115107 01 :25:01
NL:3.40E4
nvz= 159.S160.5
F: + c ESI Full ms2
293.00@15.00 [
125.00-315.001 MS
Spot10
{*,/u
(+u)
C:XcalibuA...\Spot1
02115107 01:35:53
i + c ESI
NL:0
n/z= 159.5-160.5
F: + c ESI Full ms2
?!3:339i33&t*
Spotl1
2.54E3
1
nlz= 246.5-247.5
00-l
*l
oo-l
*-l
F: + c ESI Full ms2

293.00@15.00 I
125.00-315.001 Ms
Spotl
--l
ro-.1
I
/5-l
'l*l
o
o
o
o
^^l
o
o
o
f*u
(,/ b<

Full ms2 293.00@15.00 [ 125.00-315.001
C:U(calibuA...\Spotl 2
02115107 01:46:44
':l
*.]
+ c ESI Full ms2 293.00@15.00 [ 125.00-315.00]
nVz= 159.$160.5
F: + c 951 Pr1;
293.00@15.00 [
125.00-315.001 MS
*.,
Spotl2
1.23E4
nlz= 246.5-247.5
F: + c ESI Fult ms2
2s3.00@1s.00 [
12s.00-315.001 Ms
Spot12
6
6
MS Spol12
493
6.L4
2't
330
2.88 4.5C
f* q(,
( qoo
5ULEDTA+C
Seq uence---CT_Spot_neg. sld [O pen]
:
Sample Name:
ive Blood extract
-nent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Unknown
cTo1
Inst Method
Path
U(calibu AData\EDTA\Brewer\CT_N egative
Proc Method
CalFile
u : \xca | | bur\methods\EDTA_Neg_swabs
Vol
0.000
Sample Name:
ISTD Amt
Dil Factor
0.000
1.000
Position
lnjVol
11
5.0
Level
Sample Wt
0.000
t-_
Comment
Study:
Client:
Laboratory:
Company:
Phone:
sample Iype File Name

cT02
Unknown
Samole lD
Path
01
C:
nst Method
C
U(cal
bu
U(cal ibu AData\EDTA\BreweACT_N egative
Proc Method
Cal File
Position
Samole Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
InjVol
5.0
mple Wt
0.000
*********************t************
fo
uno
(+'t)
/QY
t'"
,\tt
Sequence---CT_Spot_neg. sld [Open]

Sample Name: Negative Blood extract
"
.nent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
11
C:Xcalibu AData\EDTA\Brewer\CT_Negative
cTo3
Inst Method
C
Proc Method
CalFile
:\)(calibu r\method s\E DTA_N eg_Swabs
Sample Vol
0.000
STD Amt
0.000
*i*i*t****t*********t****ff
Position
lnjVol
11
5.0
Level
Samole Wt
u.u00
DilFactor
1.000
**********

Comment:
Study:
Client:
Laboratory:
Company:
Phone:

Unknown
cT04
Sample lD
Path
11
Inst Method
:Xcali
bu
Proc Method
r\Data\E DTA\Brewer\CT_Negative
Cal
File

Sample Vol
ISTD Amt
Dil Factor
0.000
U.UUU
I.UUU
jPosition
11
InjVol
5.0
Level
lSample Wt
10.000
-tbs
+qb
I!:?
r,\rj\"t
Seq uence---CT_Spot_neg. sld [Open]

Sample Name: JC2neg
rent:
Study:
Client:
Laboratory:
Company:
Phone:
cT05
Unknown
Sample lD
Path
02
Xcali
bu
Proc Method
lnst Method
C :U(ca libu
r\Data\EDTA\Brewer\CT_Negative
CalFile
r\method s\E DTA_N eg_Swabs
Sample Vol
ISTD Amt
Dil Factor
0.00u
O.UUO
1.000
Position
InjVol
5.u
Sample Wt
Level
0.000
t*t*********t*****************t**********************************t*****r********i**t**
Sample Name:
extract
Study:
Comment:
Client:
Laboratory:
Company:
Phone:

UNKNOWN
cT06
Samole lD
Path
11
lC:U(calibur\Data\EDTA\Brewer\CT_Negative
Proc Method
lnst Method
C
Cal File
Position
:Xcal ibu r\methods\EDTA_N eg_Swabs
sampre vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
11
InjVol
Level
tSamole Wt
0.000
i5.0
-1vP
{* uq,
(+")
nana
1\..(\'1

Sample Name:
Blood extract
rent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
11
C:U(calibuAData\EDTA\Brewer\CT tteoative
cTo7
Inst Method
:Xcal
bu
Proc Method
Position
CalFile
4a
tl
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
llnjVol
Samole Wt
Level
5.0
0.000
Sample Name: JC3neg

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
03
iCT08
nst Method
\Xcalibu r\Data\E DTA\Brewer\CT_N egative
Proc Method
Position
Cal File
v. \/\sailour\melnoos\tr u I A_Neg_
mple Vol
0.000
ISTD Amt
Dil Factor
0.000
1.U00
llnjVol
Level
;Sample Wt
5.0
0.000
Rq
q,/
b
(,/%)
n^da l
1lt(\"1

Sample Name:
extract
rent:
Study:
Client:
Laboratory:
Company:
Phone:
Samole lD
Path
Unknown
11
C : U(cal ibu
cT13
Inst Method
Proc Method
AData\E DTA\Brewer\CT_Negative
CalFile
C:U(ca libu r\methods\EDTA_Neg_Swabx
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Position
lnjVol
11
5.0
Level
Samole Wt
0.000
Sample Name: JC5neg

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
cT14
unKnown
Samole lD
05
Inst Method
C
\Xca
li b u
Path
:Xcalibur\Data\EDTA\Brewer\CT Neoative
Proc Method
CalFile
r\methods\E DTA_Neg_Swa bs
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Position
InjVol
5.0
Level
Sample Wt
0.000
l***********************t***t**************t*t*******t***********
f,(++q,
tr)
nana 7
-1rq
,\,,\"
Seq uence--CT_Spot_neg. sld [Open]
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
04
C:U(calibur\Data\EDTA\Brewer\CT
T11
Inst Method
Proc Metnod
CalFile
:U(calibu r\methods\E DTA_Neg_Swabs
Samole Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Neqative
Position
InjVol
5.0
Level
Samole Wt
0.000
********************t****t******t******a*******t
a**r*******t****r**

Comment:
Study:
Glient:
Laboratory:
Company:
Phone:

Unknown
cT12
Sample lD
Path
11
lnst Method
C
:U(calibu r\Data\EDTA\Brewer\CT Neqative
Proc Method
U(calibu Amethod s\EDTA_N eg_Swabs
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
I.UUU
Cal File
Position
11
InjVol
Level
lSample Wt
r5.0
0.000
,$e
+,/ (f*(,t1;D
, \,.(\or

Sample Name:
extract
'nent:
Study:
Client:
Laboratory:
Company:
Phone:
cT09
Unknown
Sample lD
Path
11
Inst Method
C U(ca li bu
:
:U(calibu r\Data\E DTA\BreweACT_Negative
Proc Method
Cal File
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
t.utlu
Position
InjVol
11
5.0
Level
Samole Wt
0.000
**********i**********t************************tr******************t********t*t*****************t**t*t*****t**********************************
Sample Name:
extract
Comment:
Study:
Client:
Laboratory:
Company;
Phone:

cT10
Unknown
Sample lD
Path
11
lnst Method
C : U(cal i bu
Xcalibur\Data\E DTA\Brewer\CT_N egative
Proc Method
Sample Vol
ISTD Amt
Dil Factor
U.UUO
0.000
1.000
Cal File
Position
InjVol
11
5.0
Sample Wt
Level
10.000
**a****i***t****t******t**t***********t******************tt**s*************
,/r ut
fuqau
u.' u)
-t\"\"'

rent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Unknown
11
cT15
Inst Method
C
Path
:
Xca
ibu
Proc Method
CalFile
:U(cal i bur\method s\EDTA_Neg_Swabs
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Position
lnjVol
11
5.U
Level
lSample Wt
u.000
*********************
Comment:
Study:
Client:
Laboratory:
Company:
Phone:

Unknown
cT16
Sample lD
Path
11
C:Xcalibur\Data\EDTA\Brewer\GT Neoative
Inst Method
C
Proc Method
CalFile
U(cal ibur\methods\EDTA_Neg_Swabs
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Position
InjVol
11
5.0
Level
Samole Wt
r0.000
.'ivq
Cv 44C
z\
( 47+S
)t.""''
Seq uence---CT_S pot_neg. sld [Open]

Sample Name:
nent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample
Unknown
rle Name
CT17
Sample lD
Path
06
Inst Method
C
:XcalibuAData\E DTA\Brewer\CT_Negative
Proc Method
CalFile
:\)(cali bu r\methods\E DTA_Neg_Swabs
Sample Vol
0.000
STD Amt
0.000
Position
InjVol
5.0
Level
Sample Wt
0.000
Dil Factor
1.000
*******************
****t***********r*t*********t****r

Comment:
Study:
Client:
Laboratory:
Company:
Phone:

Unknown
cT18
Sample lD
Path
11
Inst Method
C
Xcalibu AData\EDTA\Brewer\CT_Negative
Proc Method
CalFile
:Xcalibur\methods\EDTA_Neg_Swabs
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1,000
Position
InjVol
11
5.0
Lu 44b
(vts)
naaa
Level
Sample Wt
0.000
11..'"

Sample Name:l Negative Blood extract
t'
rent:
Study:
Client:
Laboratory:
Company:
Phone:

unKnown
cT19
Sample lD
Path
11
C:XcalibuAData\EDTA\Brewer\CT Neoative
Inst Method
Proc Method
CalFile
C :U(calibur\methods\E DTA_N eg_Swabs
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
Position
lnjVol
11
5.0
Level
lSample Wt
0.000
****t****t**+**************t****t*****1
Sample ttame:
Study:
Client:
Laboratory:
Company:
Phone:

Unknown
f20
Sample lD
Path
07
lnst Method
Xcalibu AData\EDTA\BreweACT_Negative
Proc Method
CalFile

Sample Vol
0.000
STD Amt
0.000
Position
InjVol
5.0
Level
Wt
i0.000
DilFactor
1.000
*******************t
[o qq,
(vto)
nana
1O
11 ,''-'

Sample Name:
extract
rent:
Study:
Client:
Laboratory:
Company:
Phone:

Unknown
Samole
'l
cT21
lD
11
lnst Method
lPath
:U(calibur\Data\EDTA\Brewer\CT Neoative
Proc Method CalFile

Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Position
lnjVol
11
5.0
Level
Sample Wt
0.000
*****tt****t**
Sample Name:
extract
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
11
C:U(calibur\Data\EDTA\Brewer\CT
CT22
lnst Method
Proc Method
Cal File
Position

Sample Vol
ISTD Amt
0.000
u.uuu
Neoative
InjVol
lLevel
5.0
lSample
0.000
Dil Factor
I
1.uuu
,sq
[) q,t,(vzt)
naaa 14
r\'(\"1
Wt
Seq uen ce--CT_Spot_neg.
sld
[O
pen]
Study:
Client:
Laboratory:
Company:
Phone:
Sample Type File
Name
cr23
Unknown
lSample lD
108
lnst Method
C :U(ca
I i
bu
Path
:U(calibu AData\EDTA\Brewer\CT_N egative
Proc Method
CalFile
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Sample Name:
Position
8
nJvol
Samole Wt
Level
5.0
0.000
ative Blood extract
Comment:
Study:
Client:
Laboratory:
Company:
Phone:

Unknown
cT24
Sample lD
Path
11
nst Method
C :U(cal
ibur\methods\EDTA_Neg_Swabs
:U(calibu r\Data\EDTA\BreweACT_N egative
Proc Method
CalFile
Position
lnjVol
11
5.0
Level
lSample Wt
0.000
{ot
f* q'/o
--(:"'^t)
L\,i\'1

lent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
11
cT25
lnst Method
:Xca
ibu
Proc Method
Sarnple Vol
ISTD Amt
Dil Factor
u.000
0.000
1.000
CalFile
Position
InjVol
11
b.u
Level
Sample Wt
0.000
Sample Name: JC9neg

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample Type File
Name
lSample lD
Path
cT26
Unknown
09
Inst Method
C
:Xcal
bu
U(cal ibu r\Data\EDTA\BreweACT_N
Proc Method
CalFile
Position
r\methods\EDTA_Neg_Sw{
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
egative
InjVol
5.0
Level
lSample Wt
0.000
'sns
4
*.,
lvtq\
'/
v\t(\"1
Seq uence---CT_Spot_neg. sld [O pen]

*nent:
Study:
Client:
Laboratory:
Company:
Phone:

Unknown
cT27
Sample lD
Path
11
C:Xcalibur\Data\EDTA\Brewer\CT Neoative
Inst Method
C
Proc Method
:U(calibur\methods\EDTA_Neg_Swa
Sample Vol
ISTD
u.0u0
0.000
Amt
CalFile
Position
njVol
Level
5.0
bs
Sample Wt
0.000
Dil Factor
1.000
*********t*********t*t************f**********************t****t*****t****t****i************t***t********t**********************i*********t*t*t
Sample tlame:
Study:
Client:
Laboratory:
Company:
Phone:

Unknown
cT28
samDle
lu
11
Inst Method
Path
C:U(calibur\Data\EDTA\Brewer\CT Neqative
Proc Method
CalFile
Position
:Xcalibur\methods\EDTA Neo Swabs

Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
11
InjVol
i5.0
Level
Sample Wt
r0.000
*i**************
-frrq
[v
aqb
(:,n.)
)\'.i
\:r

Sample Name:
0neg
rent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample Type
Unknown
ile
Narne
lSample lD
cT29
10
Inst Method
C
Path
C : U(cal
ibur\Data\EDTA\BreweACT_Negative
Proc Method
CalFile
:Xcal ibu r\methods\E DTA_N eg_Swabs
Sample Vol
ISTD Amt
Dil Factor
0.u00
0.000
1.000
Sample Name:
Position
InjVol
10
5.0
Level
Sample Wt
0.000
ive Blood extract
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
$ample lype File Name

Unknown
ample Vol
cT30
STD
Amt
Sample lD
Path
11
U(calibur\Data\E DTA\BreweACT_N eg ative
lDil Factor
I
0.000
0.000
1.000
fo
u+a
(+t,)
{1t
,t.<\r

Sample Name:
extract
rent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Unknown
11
cT31
Inst Method
Path
;
\Xcalibu r\Data\EDTA\Brewer\CT_Negative
Proc Method
CalFile
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
Position
iT-
C:\)(calibur\methods\ED1a_Neg:Swebi
InjVol
Level
5.O
Sample Wt
U.UOO
t******t***********t******t*******t************************t*t*************t***********st***********r**ti**********************r************
Sample Name: Pos. Control EDTA btood
eit
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
12
CT32
Inst Method
I
0.000
U(cali bu r\Data\EDTA\BrewerEfl*.|egaiite
Proc Method
u : \xcat bu r\methods\E DTA_Neg_Swabs
Sample Vol
STD Amt
0.000
CalFile
Position
lnjVol
12
5.0
Level
Sample Wt
10.
DilFactor
1.000
**********i**************************************t****i***t***************************i***
u'/va
!u:')
,-\!t
)\r(\-n

nent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample Type
ile Name
Unknown
Sample lD
Path
11
nst Method
:U(calibuAData\EDTA\Brewer\Spot Size_Negative
Proc Method
Position
Cal File
G:Xcalibur\methods\EDTA Neo Swabs

Sample Vol
ISTD Amt
Dil Factor
U.UOU
0.000
1.000
11
njVol
Sample Wt
Level
5.0
0.000
Sample Name: 1uL EDTA+ A

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Samole lD
Path
Unknown
13
lSpotOl
Inst Method
:U(calibu AData\EDTA\B rewer\Spot Size_Negative
Proc Method
CalFile
Position
njVol
Level
lSample Wt
I
Xcal
bu
r\methods\EDTA_Neg_Swabs
Samole Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
13
LX
UWa
(4 (")
5.0
0.000
'int
" '\a ^
..
\.s'
Sequen ce---CT_Spot_neg. sld [Open]

Sample Name:
ive Blood extract
nent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
11
C:U(cal ibu r\Data\EDTA\Brewer\Spot Size-Negative
SpotO1
Inst Method
C
Proc Method
CalFile
U(calibur\m eth od s\EDTA_Neg_Swabs
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Position
InjVol
11
5.0
Level
Sample Wt
u.000
***************
Sample Name: 1uL EDTA+ B
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
14
SpotO1
U(cali bu r\Data\EDTA\BreweASpot Size_Negative
t******r**t*********
-{$$
44t
( 4s1)
-t,ut"'
Seq uence---CT_Spot_neg,
sld [Open]
lent:
Study:
Client:
Laboratory:
Company:
Phone:
Samp
Frle Name
Sample lD
Path
Unknown
Spot01
11
C:U(cali bu r\Data\E DTA\Brewer\Spot Size_N egative
lnst Method
Proc Method
ual Frle

Sample Vol
ISTD Amt
Dil Factor
0.000
U.UUU
r.000
Position
InjVol
11
5.0
Level
Samole Wt
U.OOU
***************************t**t*****************t********t*t***
Sample Name:
Comment:
r-"'-l
Study:
Client:
Laboratory:
Company:
Phone:
Samole lD
Path
Unknown
15
SpotO1
Inst Method
:Xcali
bu
Proc Method

Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
r\Data\EDTA\Brewer\Spot Size_N egative
CalFile
Position
lnjVol
15
5.0
Level
lSample Wt
0.
'v\
' -\o
n^Cl
&( q,to
+rs)
r,\\J

('
nent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
11
Spot01
lnst Method
Xcal
ibu AData\EDTA\B rewer\Spot S ize_N egative
Proc Method
CalFile
Position
InjVol
11
5.0
Level
jSample Wt
I
Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
u.u00
.t
Sample Name:
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
to
SpotO1
lnst Method
:\)(cali bu r\Data\EDTA\B rewer\S pot
Proc Method

Sample Vol
ISTD Amt
Dil Factor
U.UUU
rJ.u00
1.000
CalFile
ize_N egative
Position
lnjVol
16
b.u
**************t*************tt****t*t*****************
Level
Sample Wt
0.000
a**************t*****
q+C2
1r^:r>
'\nR,ra
r\$'

Sample Name:
extract
nent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample Type l-rle Name
Sample lD
Path
Unknown
11
C:Xcali
Spot01
Inst Method
:
bu
Proc Method
AData\EDTA\Brewer\Spot Size_Negative
Cal File
U(calibu r\methods\E DTA_Neg_Swabs
Sample Vol
ISTD Amt
0.000
0.000
Sample Name: SuL EDTA+
Position
lnjVol
11
b.rJ
Sample Wt
Level
U.OOU
Dil Factor
t1.000
Commenl
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
17
iSpotOl
lnst Method
:Xcalibu AData\EDTA\Brewer\Spot
Proc Method
Cal File

Sample Vol
ISTD Amt
DilFactor
0.000
0.000
1.000
ize_Negative
Position
InjVol
17
b.0
&qqn
(
vsz)
Level
:Sample Wt
0.000
11,1'"

Sample.Name: Negative Blood extract
t'
nent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Unknown
11
SpotO1
Inst Method
Path
:Xcal
bu
Proc Method
r\Data\EDTA\BreweAS pot Size_N egative
CalFile
C:U(calibu r\methods\E DTA_N eg_Swabs
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Position
InjVol
11
5.0
Level
Sample Wt
0.000
Sample Name: 5uL EDTA+ C

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
18
C:Xcalibu AData\E DTA\Brewer\S pot Size_N egative
SpotO1
Inst Method
C
:Xca
ibu
Proc Method
CalFile
r\method s\E DTA_N eg_Swabs
Sample Vol
STD Amt
Dil Factor
0.000
0.000
1.000
Position
InjVol
18
5.0
(/ rl (-
(+s)
aaaa
)r)
Level
lSample Wt
0.000
1\,rJ
rr\'.
'
Seq uence---CT_S pot_neg.
sld [Open]
-rent:
Study:
Client:
Laboratory:
Company:
Phone:
Samole lD
Path
Unknown
11
Spot01
Inst Method
;
U(calibu r\Data\EDTA\Brewer\S pot Size_t tegative
Proc Method
CalFile
\Xca I I bu r\methods\E DTA_N eg_Swabs
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
Position
InjVol
11
5.0
Level
Sample Wt
0.000
****t*******************t****t**************************t*****t************t**r*********************************************r*****i*t*****i
Sample Name: 1OuL EDT

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Samole lD
Unknown
19
Spot01
Inst Method
C
Path
:Xcal
bu
Proc Method
r\Data\E DTA\Brewer\Spot
Cal File
:U(ca I i bu r\m ethod s\EDTA_Neg_Swa bs
Sample Vol
ISTD Amt
Dil Factor
U.UUO
0.000
1.U00
ize_frlegative
Position
InjVol
19
5.0
Level
Sample Wt
0.000
r*************i************
C4L
qqG
/\
(Vs'iS
st,,,..,
4/\r'
Seq uen ce---CT_Spot_neg.
sld [Open]
rent:
Study:
Client
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
11
SpotO1
Inst Method
:U(cali bu r\Data\E DTA\Brewer\Soot S ize
Proc Method
CalFile
sample vol
ISTD Amt
DilFactor
0.000
0.000
1.000
N eo
ative
Position
InjVol
11
5.0
Samole Wt
Level
0.000
***+********************t*************t*********************
Sample Name:
Comment:
Study:
Client:
Laboratory:
Company:
Phone:
Sample lD
Path
Unknown
20
Spot01
lnst Method
C
U(cali bu r\Data\EDTA\Brewer\Spot Size_N egative
Proc Method
U(calibu r\methods\EDTA_Neg_Swabs
Sample Vol
ISTD Amt
Dil Factor
O.UUU
0.000
1.000
CalFile
Position
InjVol
20
5.0
Level
Sample Wt
0.000
********************t****r
6r++t('/ q,)
{\\*.1
V\

nent:
Study:
Client:
Laboratory:
Company:
Phone:
C:Xcalibur\Data\EDTA
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.000
*************************************************************************i*********t**t************r***i******t****.****************************t
Sample Name: 1OuL EDTA+

Comment:
Study:
Client:
Laboratory:
Company:
Phone:
nst Method
Proc Method
ual Ftle
A_Neg_
Sample Vol
ISTD Amt
Dil Factor
0.000
0.000
1.U00
Position
InjVol
12
5.0
Level
Sample Wt
0.000
*****t********************t*******t****************i*******t***********t***$******i
***i*******i**********t****t*******
5r,/,/a
(\:,)
.i$$,1o1

Sample Name:
extract
'"nent:
Study:
Client:
Laboratory:
Company:
Phone:
Sample Type
Unknown
rle Name
Spot01
Sample lD
Path
11
C :U(cal ibu
Inst Method
C :U(ca libu
Proc Method
Sample Vol
ISTD Amt
Dil Factor
u.00u
0.000
1.000
r\Data\E DTA\BreweASpot Size_Negative
CalFile
Position
InjVol
11
5.0
****************
Level
Sample Wt
0.000
*************ft**#*
fi(48,v+o
1l'+^
C:\XcalibuA...\Spot Size_Negative\Ct33
02116107 03:47:38
rlz=
Negative Blood extract
TtB
NL: 1.42E3
272.5-273.5 F: - c
nvz: 299.5-300.5 F: - c
ESI SRM ms2
FSI SRM ms2

344.20@1s.00 I
299,50.300.50,
325.50.326.501 MS
cr33
29120@15.00 [
246.sO-247.50,
272.50-273.501 MS
c133
121E3
mlz= 246-t247.5 F: - c
ESI SRM ms2
291 .20@15
t5.00 [
246.50-247
246.50-247.50.
272.50-273.s01 MS
ct33
Q
d
g
@
.I]/z= 282.a-28r'.,3
ESI SRM ms2
303.20@15.00 [
282.7r2U.251
ct33
5r
F'.
-c
MS
4+o
C:\i(catibuA...\Spot01
'-1
03:58:32
uL EDTA+ A
ll
esJ
tlt
oz16t\7
I
ll
4.43E3
nlz=246.1247.5
: E.55E3
F: - c
ff|/z= 325.5-326.5 F: - c
ESI SRM msz
344.20@15.001
299.50-300.50.
325.50-326.501 MS
Spoto l
ESI SRM ms2
291.20@15.00 [
246.50-247.50,
272.50-273.501 MS
Spotol
o
6
c
q
o
nlz= 282.8-2U.3 F: - c
ESI SRM ms2
303.20@15.00 [
282.7$284.251 MS
Spoio'l
froo,
Time (min)
Time (min)
C:XcalibuA. .\Spot01_0702 1 6040921
|..--
,::
;l
02116107 04:09:21
NL:5.66E3
tnlz=272.5-273.5 F: - c
ESI SRM ms2
291.20@1s.00 [
TDp
NL: 3.2483
nvz: 299.5-300.5 F: - c
ESI SRM ms2
344.20@1s.00 [
299.50-300.50,
325.50-326.501 MS
Spot01_07021'6040921
246.fi-247.50,
272.50-273.50t MS
Spoto1-07021-6040921
mfz= 325.t326.5 F: - c
ESI SRM ms2
344.20@15.00 [
299.50-300.50,
325.50-326.501 MS
Spoto1_07021 6040921
o
o
E
c
.E
fi12.282.8-2U3
Fi - c
ESI SRM ms2
303.20@15.00 [
282.75-284.251 MS
Spoto1_07021-6040921
ffVz= 31 1.5-312.5 F: - c
ESI SRM ms2
3s6.00@1s.00 [
311.50-312.501 MS
Spoto1_07021 6040921
fo,/+,
Time (min)
C:\Xcalibur\...\Sootl1
07 021
6042017
02j16107 04:20:17
NL:2.96E4
nlz= 272.1273.5 Fi - c
NL: 3.74E4
r/z= 299.5.300.5
ESI SRM ms2

291.20@15.00 I
246.50-247.50,
272.50-273.501 MS
Spoto'l_0702 1'504201 7
325.50.326.501 MS
Spotol_07021-6042Ol 7
45
40
1.33E4
m/z= 246.5-247.5 F: - c
ESI SRM ms2
291.20@15.00 [
246.@-247.50.
272.50-273.501 MS
Spotol_07021'604201
10(
Y:
F: - c
ESI SRM ms2

344.20@15.00 [
,oa qn-ann qn
(tlz= 2E2.8-2U.3 F: - c
ESI SRM ms2
303.20@1s.00 [
282.75-2U.251 MS
spotol_07021ir04201 7
EC
ta
7A
65
DU
5C
50
45
40
30
&,%
( vt)
Time {minl
C:ti(calibuA. \Soot01 070216043106
02116107 04:31:06
Tvp
NL:0
ttlz= 272.5-273.5 F: - c
ESI SRM msz
291.20@15.00 I
246.50-247.50,
272.s0-273.501 MS
Spoto1_0702'1 60431 06
'10(
nlz= 246.5-247.5F'. - c
ESI SRM ms2
291.20@15.00 [
nvz= 325.S326.5 F: - c
ESI SRM ms2
344.20@15.00 [
299.50-300.50.
325.50-326.501 MS
Spoto1_07021'50431 06
246.50-247.50.
272,50-273.501 MS
Spoto1_07021'60431 06
da
7a
7A
8oo
o
a
F
50
V,lb
(,to)
Time (min)
Time (min)
C:U(calibur\...\S ool01 070216044202
100-.1
*t
'-l
02116107 04:42:02
u-6c
1uL EDTA+ C
-rn3
NL: 3.9'1E4
rn/z= 299.$300.5 F: ESI SRM ms2
344.20@15.00 [
z9v.JU-JUU.3U,
.riz=272.5-273.5 F: - c
ESI SRM ms2
291.20@15
| 5.00 [
246.fi-247
246.fi-247.50,
272.50-273.501 MS
Spoto1_07021'60/t4202
325.50-326.s01-60,14202
MS
Spot01
-07021
NL:'1.7784
dz:246.5-247 .5
F: - c
ESI SRM msz
291.20@15.00 [
246.50-247.50.
272.50-273.501 MS
Spoto1_07021-6044202
rvz= 325.5-326.5 F: - c
ESI SRM ms2
3,14.20@15.00 I
299.50-300.50,
325.50-326.501 MS
spot11
_070216044202
I
o
.a
6
't0(
9(
NL:4.72E4
nlz= 242.E-2U.3 Fi - c
nrlF 311.5.312.5 F: - c
ESI SRM ms2

303.20@15.00 [
282.75-284.251 MS
ESI SRM ms2

356.00@15.00 [
311.50-312.501 MS
Spoto1_07021'6044202
spoto1_07021ii044202
8(
7!
70
5C
35
30
5"w,,
(
4os)
i
C:U(calibur\...\SpotO1 _07021 6M5255
0?/16107 04:52:55
{v(,
NL: 2.67E3
nvz= 299.5-300.5 F: - c
ESI SRM ms2
344.20@15.00 [
299.50-300.50,
325.50-326.501 MS
Spoto1_0702 16045255
Etlz= 272.U273.5 Fi - c
ESI SRM ms2
2s1.20@1s.00 [
246.5G247.50.
272.5c223.s0i MS
Spot01_07021'5045255
90
80
75
70
oc
o
E
o
o
100
rlz=
282.V2E'4..3 F: -
m/z= 3'11.t312.5 F:- c

ESI SRM ms2
3s6.00@15.00 [
311.50-312.501 MS
ESI SRM ms2

303.20@15.00 [
90
282.7$2U.251 MS
spoto1_0702 1b045255
Spotol-070216045255
85
80
75
70
65
55
JU
45
40
35
JU
V46
(,+ qq)
Time (min)
0A16107 05:03:50
C:L\calibur\...\Soot01 070216050350
5uL EDTA+ A
--
00-t
(lz=272.5-273.5 F: - c
o.-l
ESI SRM msz

291.20@15.00 [
246.50-247.50,
272.50-273.501 MS
NL: 4.35E4
mh= 299.5-300.5 F: - c
ESI SRM ms2
344.20@15.00 I
299.50-300.50,
325.50-326.501 MS
Spoto1-07021 6050350
Spot0
NL:6.98E4
1
-fip
*l
".-l
0
10(
NL:1.03E4
1.06E4
.'].lz= 246.5-247 .5 F: - c
ESI SRM ms2
9:
l_0702'l 6050350
nVF 325.5-326.5 F: - c
ESI SRM ms2
344.20@1s.oo I
299.50-300.50,
325.50-326.501 MS
Spot01_07021 6050350
291.20@15.00 [
246.50-247.50.
272.sO-273.501 MS
Sootol 070216050350
8(
7,
6a
8u
o
o
a
filz= 28?.8-2U.3
F'.
-c
r/z= 311.5-3'12.5 F: -
303.20@1s.00 [
242.75-2U.25t MS
Spotol-07021'6050350
qqb
(1
Time (min)
ESI SRM msz

356.00@15.00 [
311.50-312.s01 MS
Spoto1_07021 6050350
ESI SRM ms2
Time (min)
C:l(calibur\.-.\SpotO1_07021
100-.1
*l
''-l
6051 444
02116107 05:14:44
NL: 4.06E3
nllz= 272.*273.5 F: - c
ESI SRM ms2
291.20@1.s.00 [
lvp
NL:2.56E3
299.5-300.5 F: - c
ESI SRM ms2
344.20@15
r5.00 I
299.50-300.
299.50-300.50,
325.50-326.501 MS
Spolo1_07021 605'1444
FVz=
246.50-247.fi,
272.50-273.501 MS
Spoto1_07021 6051,144
NL:0
mlz=246.5-247.5 F: - c
mtz= 325.5-326.5 F: - c
ESI SRM ms2
344.20@15.00 [
299.50-300.50.
325.50-326.501 MS
Spoto1 _07021'6051 444
ESI SRM ms2

291.20@15.00 [
246.50-247.50,
272.50-273.s01 MS
Spoto1_07021'6051444
d
c
.z
=
6
rnlz= 282.8-2U.3 Fi - c
ESI SRM ms2
303.20@15.00 [
282.75-284.251 MS
sooto1 07021tt051444
r/z=
31 1.5-312.5 F: - c
ESI SRM ms2

356.00@1s.00 [
311.50-312.501 MS
Spotol_07021'6051 444
C:\J(calibur\.,.\SpotO 1 _07021 6052539
02116107 05:25:39
5uL EDTA+ B
.----
NL: 4.47E4
NL:4.08E4
trVz- 299.$300.5 F: . c
ESI SRM ms2
344.20@15.00 [
299.50-300.50,
325.50.326.s01 MS
Spoto1_0702'1 6052539
nlz= 272.5-2735 F: - c
ESI SRM ms2
291 .20@15.00 I
246.50-247.50,
272.50.273.501 MS
Spoto1-07021'6052539
1001
e5J
no-]
--l
-jb3
NL: 1.03E4
ftlz= 246.5-247.5 F: - c
ESI SRM ms2
291.20@1s.00 I
n/z= 325.$326.5 F: - c
272.50-273.501 MS
Spoto1_07021 6052539
ESI SRM ms2

34420@15.00 [
299.50.300.50,
325.50-326.501 MS
Spoto'l_07021 6052539
mlz= 282.8-2U.3 F'. - c

ESI SRM ms2
303.20@1s.oo I
282.75-2U.251 MS
Sooto1 0702'16052539
6.80E4
nvz= 31 1.t312.5 F: - c
ESI SRM ms2
3s6.00@15.00 [
311.50-312.501 MS
Spotol-0702 1 6052539
246.50-247.50,
eo-l
I
ru-1
'"1
^-l
*l
p *-l
[,
qar-
(s"\
Time (min)
C:l(calibuA...\Spot01_07021 6053635
001
*l
oJ
'-l
0U16107 05:36:35
NL:2.19E3
nlz= 272.*273.5 F: - c
'.:fr8
NL:o
nVr
299.5.300.5 F: - c
ESt SRM ms2
344.20@15.00 I
299.50-300.50,
325.50.326.501
501 MS
ESI SRM ms2

291.20@15.00 [
246.50-247.50,
272.50.273.501 MS
Spoto1_0702 1-6053635
121 6053635
Spoto 1_0702
1.9583
mfz= 325.5.326.5 F: ESI SRM ms2
344.20@1s.00 I
zw.cu-JUu.tu,
325.50-326.501 MS
Spolol_07021 6053635
c
o
o
o
Nz= 282.8-2U.3 F: -
ESI SRM ms2

303.20@15.00 [
282.75-2U.251 MS
spot01_07021it053635
Zo't*
(sot
rvz= 311.$3'12.5 F: - c
ESI SRM ns2
356.00@15.00 I
311.50.312.501 MS
Spot0'1_07021
6053635
C:VcalibuA...\Soot01 07021 60S726
iool
"i'
'u-l
'r-J
02116107 05:47''26
5uL EDTA+ C
NL: 4.97E4
tvz= 272.*273.5
'rvp
NL:6,68E4
F: - c
rvz: 299.5-300.5
ESI SRM ms2
F: - c
SRM msZ
344.20@15.00 [
ESI
29120@15.00 [
246.50-247.fi.
299.50-300.50,
272.50-273.50i Ms
325.50-326.501 MS
Spoto1_07021 6054726
Spoto1_07021 6054726
:2.71E9
NL:6.04E9
rnlz= 246.5-247 .5 F: - c
r/z= 325.5-326.5 F:.
ESI SRM ms2
ESI SRM ms2
2e1.20@1s.00 [
246.50-247.50,
272.s0-273.50] MS
344.20@15.00 [
299.50-300.50,
325.50-326.501 MS
Spolo1_07021 6054726
Spoto1_07021 6054726
NL:6.88E5
nlz= 2E2.E-2U.3 F: - c
ESI SRM ms2
303.20@1s.00 I
2A2.75-2U.251 MS
spot0l_0702'1 i;054726
7.64E4
10(
m/2= 31 1 .5-312.5 F: - c
ESI SRM ms2
a<a n6^r < nn I
311.50-312.501 MS
Spot01_0702 1 6054726
9i
8l
7a
42
2a
2(
1l
Tlme (min)
C:l'(calibuA...\Spot01_07021
6055824
02116107 05:58:24
NL: 3.66E3
mlz=272.5-273.5 F: - c
ESI SRM ms2
291.20@15.00 [
^qjr6
NL:1.07E3
rvz= 299.5-300.5 F: . c
ESI SRM ms2
344.20@15.001
299.50-300.50,
325.50-325.501 MS
Spot01 _0702'l'6055E24
246.fi-247.50,
272.50-273.501 MS
Spoto'l_07021'605582,1
NL:4.15E3
mlz= 246.5-247 .5 F: - c
ESI SRM ms2
291.20@15.00 [
r/z= 325.5-326.5 F: - c
ESI SRM msz
344.20@15.00 [
299.50-300.s0,
325.50-326.501 MS
Spoto1 _07021'6055824
246.50-247.fi,
272.50-273.501 MS
Spoto l_07021 6055824
I
o
10{
=282.+2U3F:
-c
ms2
D15.00 [
284.251 MS
070216055824
8{
7!
7(
b:
5:
5L
35
3C
44a
(*')
NL: 3.1 5E3

mfz= 31 1.5.312.5 F: - c
ESI SRM ms2
356.00@1s.00 [
311.50-312.501 MS
Spoto1 _07021'6055824
02116107 06:09:17
C:XcalibuA...\SootO1
NL: 1.29E5
ntlz= 272.5-273.5 F: - c
ESI SRM ms2
291.20@15.00 [
"it
'ol
,u'l
'o-l
ll
lOuL EDTA+ A
m/z= 299.t300.5 F: - c
ESI SRM ms2
344.20@15.00 I
246.50-247.fi,
299.50-300.50,
325,50-326.501 MS
272.s0-273.501 MS
Spoto l_07021 606091 7
Spoto1 _07021606091
NL: 1.2484
nlz= 246.5-247 .5 F: - c
ESI SRM ms2
291.20@15.00 [
246.50-247.50,
272.50-273.501 MS
Spoto l_070216060917
1.66E4
ruz= Jl5.+JZb.a f :- c
ESI SRM ms2
344.20@15.00 [
299.50-300.50,
325.50-326.501 MS
Spoto1_07021 60609'l 7
o
6
E
.!l
E.
nlz=242.&2U.3 F: - c
ESI SRM ms2
303.20@15.00 [
282.75-2U.25) MS
Spol01_07021 606091 7
fo qqb
(s4
Time (min)
llu/'
Time (min)
C:\j(calibur\...\SpotO1_07021 606201
1001
*l
oo_J
02116107 06:20:13
NL:2.74E3
fitlz=272.5-273.5 Fi - c
ESI SRM msz
nvz= 299.$.300.5 F: - c
ESI SRM ms2
344.20@15.00 I
299.so.5oo.so,'
325.50-326.501 MS
spoto1_0702'tb062o.t 3
291 .20@15.00 [
246.50-247.50,
272.50-273.501 MS
Spot01_07021 606201 3
1001
9fl
I
s0-l
*l
qa-l
TNB
rnlz=246.5.247.5 F: - c
ESI SRM ms2
291 .20@1s.00 [
246.50-247.50.
272.50-273.soi Ms
Spotol_07021 606201 3
roJ
rr-l
to-l
es-]
60--1
cd
nlz=282.8-Z8/..X F: - c
nfz=
ESI SRM ms2

303.20@15.00 [
31
1.9312.5 F: - c
ESI SRM ms2
356.00@15.00 [
311.s0-312.501 MS
282.75-2U.251 MS
Sootol 070216062013
L/
Spoto1_07021'606201
tl
(t.t)
Time (min)
02116107 06:31:08
:\Xcalibur\...\SpotO1 _07021 60631 08
..,------
1oo-l
'i'
"-lil
^!il
1001
*t
qr-.1
so-l
--i
NL; 8.64E4
mlz= 272.5-273.5
'
F'.
-c
ESI SRM msz
29r.20@15.00 [
246.50-247.50.
272.50-273.s0i Ms
299.50-300.50.
Spoto1_07021 606310E
Spoto1_07021'6063
NL: '1.03E4
trlz=246.*247.5F:-c
ESI SRM ms2
291.20@15.00 I
246.50-247.50,
272.50-273.50t MS
Sooto1 070216063'106
80-]
I
tu-]
rol
oc-1
n/z= 299.5-300.5 F: - c
ESI SRM ms2
344.20@15.00 [
.o-l
.rJ/z= 242.8-28/..3 F: - c
ESI SRM ms2
303.20@15.00 {
2A2.75-2U.251 MS
Spoto l_07021 60631 08
&.
(
+vro
s"r)
325.50-326.501 MS
1
O8
:!Xcalibur\-..\Spot01_0702
6064204
02116107 06:42:04
-T1)a
NL:6.39E3
100-.]
*l
'I
rnlz=272.?273.5F: - c
ESI SRM ms2
2e1.20@15.00 [
246.fi-247.50,
272.50-273.501 MS
Spoto1_07021'6064204
nlz=246.5-247.5 Fi - c
r/z=
325.5-326.5 F: - c
ESI SRM ms2
344.20@15.00 [
299.5G.300.50,
325.50-326.501 MS
Spoto1_07021'6064204
ESI SRM ms2

291.20@15.00 [
246.fi-247.50.
272.50-273.501 MS
Spoto1_07021 6064204
o
o
NL:4.2482
ff'lz=282.*2U3F.ESI SRM ms2

303.20@15.00
282.75-2U.251 MS
Spol01_07021 6064204
m/z= 31 1.5-312.5 F: . c
ESI SRM ms2
356.00@1s.00 [
311,50-312.501 MS
Spoto1_07021 6064204
C:LXcalibur\...\Spot01 _0702 1 6065301
02116107 06:53:01
.lj/z=272.5-273.5F: - c
ESI SRM ms2
2e1.20@15.00 [
246.50-247.50,
272.50-273.501 MS
Spoto1-07021'6065301
NL: 1.42E5
miz= 299.5-300.5 F: - c
ESI SRM ms2
344.20@15.00 [
299.50-300.50,
325.50-326.501 MS
Spot01_0702 1 6065301
nz= Jz5.'Jzb.5
*l
o.-l
F:
.c
ESI SRM ms2
344.20@15.00 [
299.50-300.50,
325.50-326.501 MS
Spot01_0702'16065301
*-l
*.1
I
^-l
ro-]
ru-l
lOuL EDTA+ C
*-1
mlz= 282.*2U.3 F: - c
ESI SRM ms2
303.20@1s.00 [
282.75-2U.251 MS
Spot01-07021-6065301
Oqv
(t,")
C:'Xcalibur\...\SootO1 07021 6070351
t*r
ni
.oJ
02116107 07:03:51
ltD6
NL: 1.71 E3
rniz= 299.9300.5 F: ESI SRM ms2
344.20@15.00 I
r,1z= 272.5-273.5 F: - c
ESI SRM rl.s2
rrls2
291.20@15
r5.00 [
246.50-247.50.
246.50-247
272.50-273.501 MS
Spoto1_07021-6070351
299.50-300,s0.
325.50-326.501 MS
Spoto1_07021 6070351
NL:5.93E3
r/z= 325.$326.5 F: - c
ESI SRM ms2
ESI SRM ms2

34420@15,00 [
299.50-300.50,
325.50-326.501 MS
Spoto 1_07021'607035'l
291.20@1s.00 [
246.50-247.50,
272.50-273.501 MS
Spoto1-07021'6070351
4.50E3
nvz= 31 L5-31 2.5 F: - c
ESI SRM ms2
356.00@15.00 I
311.50.312.s01 MS
Spot01_07021 6070351
mlz=282.&2U3 Fi - c
ESI SRM ms2
303.20@1s.00 [
282.7t2U.251 MS
sootol
07021b070351
6" ++
(s
t,)
i
TM IDIAGNOSTICS
t"
4*u
i rz-r)
C:U(uElibur\...\EDTA\BreweA021
100 ppm EDTA tm
507U1 501
r#sE RT:0.79 AV:
+ c ESI Full ms2 293.00@15.00 [ 125.00-315.001
t::
nlz=246.1247,5
t"t
*l
F: + c 951 Pr',
293.00@15.00 I
ro-l
21501
125.00.315.00t MS
ru-]
ro-]
tul
^-l
6s-1
o ^^l
s, ."1
'^/
'\*iJruqMA
,,, A
"'vV YV\,ry'\,\
^
[<. aa
(
<,t
ClXcelibuA...\EDTA\BreweA02
307U1 302
0U13107 08:50:58
-l?p
100 ppm EDTA
NL: 1.06E5
nvz= 299.5-300.5 Ft . c
ESI SRM msZ
344.20@1s.00 [
299.50-300.50,
32s.50-326.501 MS
21302
ED'fFronl
r/z= 325.t326.5
Fi - c
ESI SRM ms2

344.20@15.00 [
299.5G300.50,
325.5G326.s01 MS
21302
o
o
o
E
o
o
rnlz=282.E-2U3F:
-c
ESI SRM ms2

303.20@1s.00 [
282.7r2U.251 MS
21302
21302
f*
Time (mrn)
m/z= 311.t312.5 F: - c
ESI SRM ms2
356.00@15.001
311.50-312.501 MS
,/r/
(*\
'
:L\calibur\...\EDTA\Brewe
rl}ZlzdlUlZ}i\t
0?/1407 02:33:58
NL:2.87E5
fiVz:159.$160.5
F:+cESl Fullms2
293.00@1s.00 [
125.0e315.001 MS
21206
rol
rul
"-l
811
NL:5.52E4
r.lz=246.*247.5
F: + c ESI Full ms2
293.00@15.00 [
125.00-315.001 MS
21206
eo-l
'J
--l
^J
o ^^l
"*l
NL: 3.71E5
Ms 21206
Ttc
f*+
(<,)
(\---tOO ppm EDT]) 76.r
+ c ESI Full ms2 293.00@15.00

[ 125.00-315.00]
\21203 07021209391
NL:3.39E5
mlz= 272.5-273.5 F: - c
ESI SRM ms2
291.20@15.00 [
246.50-247.50.
272.50-273.501 MS
21203 070212093914
\6e
L: 1.30E4
mlz-- 246.5-247.5 F: - c
ESI SRM ms2
2e1.20@15.00 [
246.50-247.50,
272.50-273.501 MS
21203_Q7021 209391 4
o)
o
o
_g
q)
E,
TIC MS
21203_070212A93914
fo ngt
(*u\
%
1q
Time (min)
123
;:J_^
2,35
135
2.SB
147
2.81
c:\Xcatibur\..Q{!1-o7o20s0sl 3d}'\
0?/09107 09:13:09
QsD
Full ms2 293.00@15.00 [ ]2s.00-315.001
r/z= 159.$160.5
F: +
c ESI Fullms2
293.00@1s.001
125.00-315.001 MS
20901_o7o2oEo91 309
NL:0
fflz= 246.*247.5 F: +
c ESI Fullms2
2s3.00@15.00 [
12s.00-31s.001 Ms
20901_07020fu9,1309
!,
o
o
E
o
':
E
o
trr/z= 157.$'168.5 F: +
c ESI Full ms2
305.00@15.00 [
125.00-315.00t MS
2090 1_07020sh91309
r: + cESt rulinilisS.ooqnd.bb iizs.obnri.obf
rnlz= 258.t259.5 F: +
c ESI Full ms2
305.00@1s.00 [
125.00.315.00t MS
20901_0702orh91 309
:3.06E4
TIC MS
2090 1_070209091 309
4q
({,')
-fpn
/\
:\XcalibuA...\EDTA\Brewer\02090iw91
02109107 09:17:22
NL:5.65E5
nr/z= 159.S1605
F: + c ESI Full ms2
:,1
293.00@15.00 [
125.00-315.001 MS
20902
:3.81E4
li:,lz=246.+247.5
F: + c ESI Full ms2
293.00@15.001
125.00-315.001 MS
20902
o
G
:3.47E3
rn/z= 167.$168.5
F: + c ESI Full ms2
305,00@15.00 [
125.00-315.001 MS
20902
rrz= 258.5-259.5
F: + c ESI Full msz
305.00@1s.00 [
125.00-315.001 MS
20902
o
o
o
G
100-l
:4.57E5
Tlc MS 20902
qnl
--l
.ol
.^l
:^.1
*-l
--.1
f,*u{
(
srt)
-trF
C:\Xt]alibuA...\EDTA\BreweAO2090700903
0209107 09:25:27
NLr 4.38E5
nVz= 159.5-'160.5
(sss
onm each EDrA, d12
+ c ESI Full ms2 293.00@15.00 [ 125.00-315.00]
'::l
F: c ESI Full msz

293.00@15.00 [
125.00-315.001 MS
20903
-.]
: 4.'19E4
rnlz=246.*247.5
F: + c ESI Full ms2
293.00@15.00 [
125.00-315.001 MS
20903
o
o
p6
o
o
o
6.67E5
m/z= 167.$168.5
F: + c ESI Full ms2
305.00@15.00 [
125.00-315.001 MS
20903
10or
*-]
.o-l
.el
,O-l
'E
C903#6&71 RT: 0.66.0.91 AV: 3 NL: 6.70E5

: + c ESI Full ms2 305.00@15.00 [ 125.00-315.001
.o
168
e
830
20
ruz= z5d.+4Y.c
F: + c ESI Full ms2
305.00@15.00 [
125.00-3'15.001 MS
20903
o
o
6
a
o
.o
foq
(sre)
Time (min)
EDTA
)U., -.)
J 9f
C:rXcalibuA...\EDT
02109107 09:48:42
NL:
+ c ESI Full ms [ 1 00.00-450.001
J.OOEf
m'Jz=
1001
--l
100.0-
ooJ
450.0 MS
20907
221
1.73
287
?.24
9F
94-
90-
8988a7-
ilt
AF-
2le
85E4A?-
a2-
818061
0.4r
797A-
45
I
76/c-
74-
o
o
72-
,-
o
o
&,
@v@
02109107 09r59:35
C:B(calibur1...\EDTA\BreweA0209o(999)
Rn{-I6:
NL:0
( eorn neg swab (2tzo7i,1

\-------.-
+ c ESI Full ms2 293.00@15.00 [ 125.00-315.001
nVz= 159.$160.5
F: + c ESI Full ms2
293.00@15.00 [
125.00-31s.ool Ms
2090E
rn!z= 246.$247 ,5
F: + c ESI Full ms2
293.00@15.00 [
125.00-315.001 MS
20908
o
o
o
E
o
:1.23E4
1675168.5
r/z=
F: + c ESI Full ms2

305.00@15.00 [
125,00-3'15.001 Ms
20908
w6*IS-1o t(t:U.9/{r.99 AV: Z NL: t.t9E/t

+ c ESI Full ms2 305.00@15.00 [ 125.00-315.00]
74
0.97
I
,l
o
o
6
6
o
o
167
3.44E4
MS 20906
z.za
Z.E
72
0.94
I
lzo
479
{n lvu
( sat)
Tlme (min)
J e(t
C :\Xb libu
r\...\EDTA\BreweA02O907@
OAOglO710:10:53
FT-030.-i
rn/z= 'l 59.5-1 60.5
F: + c ESI Full ms2
293.00@15.00 [
125.00-315.001 MS
20909
:7.09E3
rVz= 167.5-168.5
F: + c ESI Full ms2
?33:3&@.13193tu'
20909
NL: 2.E'1E3
nl/z= 258.$259.5
F: + c ESI Full ms2
305.00@15.0O I
125.00-315.001 MS
20909
t.
lq
IE
to
I<
lo
l6
7.s3Es
Ms2osos
6uo')
&rl
I
0909#6E-76 RT: 0.90-0.98 AV: I

: + c ESI Full ms2 293.00@15.00 [
NL:9.35E5
,9
C:\i(calibur\...\EDTA\Brewer\020907Q0910
oztogloT
:417
i.ils
lO:27:12
(tomy1y@
5P
lT: + c ESI Full ms [ 100.00450.00]

NL:
7.24Et I .^^
168
TIC MS
20910
94-
929190-
8E-
87E6-
t<84-
243
q?8281-
5l
35 -;-
214
1.57
8079t6-
I)74-
73-
o
o
'a-
6
E
o
o
G
t"u
(Ea)
*1
o'5,
oot',
REFERENCES
to+,to
(<^+)
Joumal of Analytical Toxicology, Vol, 21, November/December I 997
The Analysis of EDTA in Dried Bloodstains by

1
Electrospray LC-MS-MS and lon Chromatography-
r
L
t:
1f
1t
tl
Mark [. Millerl, Bruce R. McCordl, Roger Martz2, and Bruce Budowlet.

tForensic Science Research and Training
Center, FBI Labotatory, Quantico, Vrginia 22135 and zChemistryIoxicology L)nit,
D.C. 20535
FBI Laboratory, Washington,
of
ro
evidence
screening
to
was
tiquid
..
Analytical methods were developed to determine the presence

ethylenediaminetetnacetic acid'(EDTA) in dried bloodsrains
provide probative information when allegations of
tanpering have been made in criminal cases. A simple
method using ion chromato6nphy to analyze slains was found
be quantitative to lhe 5 ppm level. The presence ofEDTA
then confirmed usingnegative and positive ion mode
chmmatography-tandem mass spectrometry (LC-[tsMS)
ff*ttl|ii,*ill*T"L'$:|,ofi"1:"T[li?,"'il:o't
proexculcrime
scenes. Allegations of "planting" blood evidence from col-
criminat
deter-
lected reference specimens has occurred in some

investigaiions, and this issue may be resolved by the
ordiacid (EDTA, also known as
mination of exogenous components that would not
narily be present in authentic crime scene
evidence.
(Figure
specimens, can be used to implicate the origin of a dried bloodC 1eH16N20s,
'.ilui,ir',r.tes
i:ill[Jr,?Lffiflj.,,:'J,ffi[i$:1?",:""f1,.1ffi1;
The collection of blood at crime scenes and for legal

ceedings is a common practice used to inculpate or
pate individuals associated with evidentiary blood at
Ethylenediaminetetraacetic
does decarboiylate when heatel to temperatures of l!g"C

(I). lt is an excellent comprexing agent and forms waterwith neaity auieavy metars. Thererore,
employ reversed-phase ion-pair liquid chromatography (LC)

for analysis of EDTA in foodstuffs (2,3), water (4,5), radioactive waste (6), and pharmaceuticals (7), Gas chromato-
rntroduction
edetic acid,.
it
exhactions of dried bloodstains should readity isons'ults aqleous

lateÊ-DTA in solution.
il;-'contamination . IDTA is used as a chelating agent in a variety of materials, and several chromatographic methods have been
bc
developed for its determination. A number of the methods
the
preservative EDTA. one intensting observalion in these

was the adsorption and postanalysi-s release of EDTA i"
chromatograpiic system. In order to avoid cros
of samplei resulting from this phenomem, it was found to
necssary to use EDTA-free blood extracls as btanks in
[C-MS analysis of
bloodstains.
blood that behave as catalysts and/or cofactors,

EDTA-preserved blood tubes use the salt forms of EDTA:
the disodium, dipotassium, or tripotassium salt, The concentration of EDTA in its free acid form in a drawn blood
tube is 1000-2000 mg/L (ppm), depending on the volume of
blood and the capacity of the tube. The free acid and salt
forms are all water soluble at this concentration. EDTA is
stable on storage and on boiling in aqueous solutions, but
molecular weight,292.24)
l), a chemical commonly added to collected blood
(lC) is an additional logical approach for the analysis of

EDTA (6). All of the previously mentioned LC methods use
ultraviolet detectors and lack the specificity of liquid chromatography-mass spectrometry {LC-MS). An additional
level ofselectivity in the analysis of EDTA can be added by
the use of LC-MS-MS. A simple extraction technique coupled with positive ion and negltive ion LC-M$-MS methods
was developed for the analysis of EDTA in preserved dried
bloodstains. Pneumatically assisted electrospray (ES) was
used to ionize the chromatographic efflueni before mass
spectnl analysis of the charged species. A secondary method
using ion chromatography was devetoped to provide a quantitative presumptive test for the presence of EDTA as will as
corroborate the results of the LC-lvlS-MS analysis. In a
blind trial conducted on 42 bloodstains using it',
tube.
rim
lhe extraction protocol for IC and LC-MS-MS;problems
_occurredintheLC-Iv1S-Iv1Sanalysis.Subsequently,a
stain as coming from this type of preserved specimen

The purpose of the EDTA in the tube is to prevent
lation and enzymatic degradation by chelating metals in
coagu-
llll;.1?::iil:Ttr'#1,'::::Hil1::,ffi:iffff,#f"T9,,,
atdincluiondcndimptyendffirnbythcFcdart Burcauoltrunisarim.
refined extraction method was developeo ror
analySiS Of
4"1 44b
Reproduoion (photocopyint) of edito{ial
."(.ff,r?),"a1
dfigd
is prohibired
blOOd.
wirhout pubtisher's permission.
rb_usjr,ri
loumal ofAnalytical Toxicology, Vol. 21, November/December 1997
;xperimental*
.tl2For the initial study, 25 to 5096 of the stained area (up t0
cut out of the cotton swatch. The cutting wai

placed,in 50 or 100'pL of 0,02SM copper (il) sulfate
cm2l was
Chemicals
American Chemical Society reagent-grade ammonium

hydroxide, disodium EDTd cupric sulfate, and high-perfor.
mance liquid chromatography (HPLC)-grade acetonitrile were
purchased from Sigma Chemical (St. Louis, M0), HplO-grade
methanol was obtained from EM Science (Cibbsto,vn, NJ).

Certified sulfuric acid (2.5M) and sterile Vacutainer blood tubes
without additives (red top)and with EDTA (K3) (lavender top)

were obtained from Fisher Scientific (Fairlawn, NJ). Nanopure
water from a Barnstead (Dubuque, IA) water purification

system was used for sampla and mobile phases. The deuterated
standard of EDTA-dp (Figure 1) was purchased from Cambridge Isotope Laboratories (Andover, MA).
Instrumentation
Ion chromatographic analysis was carried out using a Waters
510 HPLC pump (Milford, MA) coupled to a Hamilton (Reno,
column, sample detec-
$UtgRAlg0#Lchromatoeraphic
ruon was perrormed us'fi'g; bpectroflow-273 tunable

absorbance detector (Kratos Analytical Instruments, Westwood, NJ.) Instnrment control and signal procasingwere per.
formed using a Millenium 2010 chromatography manager
(Waten, Milford, MA), Additional ion chromatographic analyses
'lere performed using a Waters 600 analytical HPLC

coupled to
Waters 990 photodiode array detector.
The LC-MS-MS work was performed on a Hewlett-Packard

(Palo Alto, CA) HP 1090 ternary LC with autosampler con.
nected to a Finnigan MAI (San Josd, CA) TSQ 700 triple*tage
quadrupole MS using a Finnigan electrospray interface. Argon
was used as a collision gas for MS-MS. The instrument was set
up to scan the mass nnge in 0.5-2 s. A flow rate of 0.3 mUmin
was used on a Hamilton (Reno,
PRP-I polymeric column
(2.1 x 150 mm).
Procedure
Test samples were made by drawing whole blood sam-
ples into unpreserved and EDTA-containing tubes, The

bloodstains were prepared on the same day by applying
between 2 and 50 pL ofunpreserved or EDTA-containing
blood onto sterile cotton Iinen. Additional sarnples were
prepared using liquid whole blood from a laboratory

volunteer.
(enough
.to _cover sample). The samples were soaked in
solution for 3 or more hours before vortex mixing and centrifuging at 3000-9000 rpm for l0 min. After passing the
gmqle through a 0.2-pm nylon syringe filter, injections oi
25 pL were made for lC analysis, The IC mobile phase
was
3mM sulfuric acid/methanot (g5:5). The flow rate was

2 mUmin with a detector wavelength of 25{ nm. This wave.
length was. subsequently changed following analysis by
a
UV photodiode array detector that indicatea fne pea[
absorbance maximum for the copper/EDTA complex occurs
at 243 nm. Following IC, the residual copper extract samples were diluted with 25 pL ofwater and l-pl injections
were made for positive ion LC-MS-MS. This preparation
method was used for all IC analyses and for thi initial run
by LC-MS-MS of the 42 blind trial samples. Subsequenr
LC-MS-MS analysis samples were prepared by the proce_
dure given in the next paragraph.
A different extraction procedure wai*developed for
LC-IIS-MS analysis to eliminate copper (ll) sulfate, which
caused arcing problems in the electrospray interface, from the
extnct. This procedure was used t0 prepare samples for both

negative and positive ion LC-MS-MS but not IC analpis. A
portion (up to l/2 cm2) of the bloodstain was extracted bv
lournal of Analy
'Results
and
lt
i*
A revlew 0l
:.
grapnlc appro
.,
,,lC analysis ot
copper or iror
"'this analysis
llsample deriva
56
inserting the sample into Millipore (Bedford, I'4A) Ljltrafree-Mi
centrifugal filters made of a polysulfone membnne (type

PTTK) with a nominal molecularweight cutoff of 30,000 DiL
tons. AIter the addition of 25 pL of water, the sample was
allowed to sit at room temperature for 45 min. The filter tubes
were centrifuged for approximately
l0 min, and the filtnte
was collected for analysis.

Positive ion LC-MS-MS data were collected by scanning for
product ions of (M + H)+ at 293 u from 12&296 u at a collision
offset of-20 V The interface was set for a spray voltage of4 kV,
a sheath gas pressure of 90 psi, and an auxiliary gis flow of
5 units. The interface capillary was maintained at 200"C. A

mobile phase of acetonitrile and water (S:95) with 0.06%
ammonium hydroxide was used.
Negative ion LC*MS-MS data were acquired by scanning
for the 300 u product ion from the iron adduct of UOtl at
344 u. A scan window of 29&302 u was emptoyed. The collision offset for selected reaction monitorin{ of the 44 u
mass loss was 20
6.5
ac
o
V The interface was ieT6r aiptay voltage
of 4.5 kV a sheath gas pressure of 50 psi, and

an auxiliary gas flow of 5 units. The heated
capillary was set for 200"C. The optimizedcolumn mobile phase for negative ion was
found to be acetonitrile and water (80:20) with
0.03% ammonium hydroxide.
The isotopic pattern calculation was per-
5.5
formed on the ChemPuter from the Department
of Chemistry at the University of Sheffield,

Figure 1. Structures, formulae, and molecular weights for EDTA and EDTAdl2,
'Thf wb .ddr6r for tfE Chefipuler is hnp.//ffi,sh{&.uw-chcny'cfrmplrcrtElop6.hht,
tJtlb
Sheffield, Englandt, The experimental isotope

pattern was calculated by adding six scans
together and the same number of background
scans were subtracted to obtain the result.
Fi6'ure
2. lo
E0TA-preset
rr/December
of Analytica I Toxicology, Vol.
1, Novemlrer/December
997
f{l
ed area
.rtting
)s
,04
nng andi
r passing
injection
ile phase
ow rate
n. This
analysis
ed the
lii{
w"
ts and Discussion
A review of the litenture indicated that ttre best chromato
J '
- I l- -rt
approach for the determination
of EDTA used HPLC or
analysis of colored complexa formed between EDTA and

or iron (2-6). Although procedures uist for performing
analysis by GC, thae methods rcquire time-consuming
le derivatization and are prone to matrix interferenca (3).
nt applications published by Hamilton indicated acceptseparations of EMA+opper complexes could be canied
using the ion exchange column PRP X-100 with sulfuric
acid/methanol mobile phases (8). Initial IC tating with W

detection was carried out on standard samples of S0-100 ppm
(lI) sulfate. The results with

this eluent system were encounging; therefon, further tests
EDTA disolved in 0.025M copper
were
out on samples of liquid blood. IC samples were pre-
pared from 200 pL of whole blood (EDTA preserved) by fint

diluting il to 2 mL with water and then diluting *re solution
with 0.05M copper (ll) zulhte. This prepantionwas centrifuged
for 7 min, which left a clear supernahnt with a brown preripitate at the bottom. A large orcas of copper (II) sulfate helped to
ensure conversion of all free EDIA to the copper complet The
l:l
nplex
extract
tL ini
prepar
re
carid
i!.i
ffi
,.q
}i
ii
F
o
veloped
300'000
from
:les for
.rce,
200,000
:xtracted
100,000
brane
400
'le
0.2 4.4 0.6
ule ll
0.8
1.2
1.4
1.2
1.4
Time (mln)
canning
500,000
ta
of4
gas flow
200"c.
400,000
ith
'scann
fEDTA
l.
fl
400,000
rlfate,
'1
ri
the
age
tii
initial
^"
":
,$
ili
500,000
Su
Y
i&l
.B
6
300'000
The
the 44
2o0,oo0
ry vol
) psi,
re hea
100,000
'timi
ion
;20) '
;20)witB
d
il
0 0.2 0.4 0.6 0.8 I
.vas pei,!
rartmer{
:effield
isotonr{
scaru:
02468
Tlme (mln)
Iime (mln)
Figurc 2. lon chromatograms of a 50 ppm EDTA standard (A) and an
EDTAareserved blood extracl (B) at a detection wavelength of 254 nm.
Figure 3. EDTA analysis of the proton adduct ion rnlz 293 by positive ion
full scan LC-MS-MS. Reconstructed ion chromatogram (solid line, scan

range 128-296 u) and EDTA product ion rnlz 160 (dashed line) traces
from unpreserved (A) and EDTA-preseved (8) blood stain extracts,
,lourna I of Ana lytica I Toxicology, Vol. 2 t, November/December

I 997
result of this analysis is shown in Figure 2. Similar analyses

using FeCl3 and Fe2(S04)3 to complex with EDTA did not pre
duce precipibtes and showed large interfering peal$. fu a resulf
all further tests were performed using Cu(lI) sulfate at a concentraiion of 0.025M in each sample. In a set of serial dilutions
in water; the analysis wu shown to have a linear nnge from zero
to greater than 500 ppm EDTA with a minimum detectable
quantity of 5 ppm EDTA for the injected sample.
A Hamilton PRP-I column was used to sepante EDTA

for MS
detection in order to reduce interference from other
coml
pounds in the blood. Other blood components were

retarded on
the column and minimized peak overlap with EDTA which

has a short retention time. IC mobile and stationary phases
were not used for the MS procedure because of the strong
buffer ion concentrations required for ion exchange that
led io
elechical arcs in the electrospray interface. An additionar reason
100
80
Eaa
EOU
0,
.g
-l
840
20
130 150
190 210 230
170
250
mh
Figure 4. Positive ion
LC-MIMS product spctrum from collision-induced dissociation of
OO
ilii
HoC-cq\.H
n/zzg3.
o
tl
HOC-CFtz\
/cft-'bon
__+
?N-c'.h-o-rr-Ni
.,t-,1o"
'of"*
o
EDTA ion (M+H)+ at
m/2p93
./
noc-ct{/
N-H "
CFh
tl
rn/z 160
fo
t"u)Lo
"t\EN-clt-clt-N\
Hoc.c/
o
ll
tcq-coH
m/z
247
HqCH
/ct+z-o$
co + cFl=61;-'\*-.o,
-il
ny'z1\2
o
'
Figure 5. Fra8rnents observed by collision-induced dissociation

preserved
blood.
/ gty\
"tt^f^{"ucr
ion(m/2293) in posirive ion
LCrvlMS
analysis of EDTA,
f:i::)'.
T
11"',r:,;
l:ttt.
)*
:,ffi
l6urnil of Analytical Toxicology, Vol. 2l , November/December
997
for keeping the ionic shength of the mobile
higher ion concentrations may suppress analyte ionization (g).

Standard sample solutions (10-100 ppm) of disodium EDTA
in water yielded abundant adduct ions by electrospray sample
phxe minimized
is
,i
i
:, loop injection (flow injection analysis, FIA) or Li-ltS in ine

positive ion mode. However, analysa of disodium EDTA with
or without chromatography gave variable spectra as a result of
;:, the formation of numerous metal complues with EDTA The
' DDTA adduct ion (lvl + H)+ at mlz 293 was observed even
' though the mobile phase was alkaline. Other charged species
observed in standard sample solutions and their proposed
identities were as follows: mlz 3I5, (M + Na).; m/23!7,
(M -2H+dlttt;-. mlz 337 , (M - H + ZNal+; mlz 346, (M 2H +
Fettt)+; mlz 368, (M - 3H + Felll + Na )*; and mlz jgl, (M - 4H
+ Feill + 2Na)*. The electrospny interface is constructed of
stainless steel and aluminum and accounts for the presence of
Felil and Allll complexes in analysa of disodium EDTA. The
electrolytic nature of electrospray has been shown to form
iron complexes from the stainles steel spny needle (10).
Negative ion FIA-MS (sample loop injection)or LGMS genented several ions with sampla of disodium EDTA including
(l'l-H)- at mlz 29I and the doubly charged ion (M - 2H;-z ut
mlz 145. Adduct ions were also observed in negative ion mode
with the same metals (pstll and Alllt) as pbsitive ion mode.
Complexed species indicated from FIA-MS or LC-MS and their
proposed identities were: mlz 313, (M - 2H + Nah m/z 315,
(M - 4H + Alrr)- mlz 335, (M - 3H + 2Na)-; and mlz 3M,
(M - 4H + Fer)-. The negative ion spectra were also poorly
reproducible in the relative intensity of the various ions for
siandard runs ofdisodium EDTA,
Positive ion LC-MS was also oramined using a series of mixtures of acetonitrile and 0.06% ammonium hydroxide. The
mobile phue (5:95) was selected as it gave the best response
masses 132
nd247 u (Figure
4). The three-product ions (132,
their associated losses are coruistent with the

known EDTA{12 spectrum which has product ions at mlz 140,
160, 247) and
168, and 259, respectively (Figure 5). The neutral losses cor.
respond to carbon monoxide, a di-carboxylic acid secondary
amine, and formic acid.
A blind trialof the analysis procedura was performed independently by IC and by positive ion LC-MS-I"1S. Forty-two
dried bloodstain extncts prepared for IC analysis were analyzed
in the blind study to determine if BDTA preserved btood could
be distinguished from unpreserved blood spots. Although the
samples were diluted with 25 pL of water before LC_MS_MS,
some electrical arcs still occurred in the elecbospray interface
(ll) sulfate in the samplej. Tire volume

of the original bloodstain samples ranged from 2 to 50 pL.
Although all stains containing EDTA (n 2l) were correctlv
=
because of the copper
identified using the IC technique, LC-MS-Mscorrectly determined 20 of the 2l positive samples, Both techniques correctly identified all of the negative samples (n Zli. A stain
=
sample that gave a positive result in the IC test had indications

of DDTA by the LC-MS-MS procedure but was considered too
weak to be called positive on a single resull This was an extract
of half of the smallest EDTA blood spot (2 pL) in the 42 sam.
ples (i.e., approximately t UL). At the time of the testing all

other positives gave significant area counts (several hundred
thousand) for the 160 u product ion, and both 132 and 24? u
ions were present. The false-negative result lnd an area count

of 80,000 for ion 160, and both other product ions were present. A conservative decision was made to interpret the sampte
as negative until further testing could be completed.
A revised extraction method was dewloped for LC-MS-MS
after the initial testing to eliminate the cupric sulfate-induced
arcing problerns in the interface and to obtain more concenand consistency for 0DTA analysis. This mobile phase gave
trated sample extracts. A simple procedure was devised to
(M + H). ions atmlz293 for the disodium EDTA standard (10
extract the stains in centrifugal filters after a A5-min soaking
to 100 ppm) and was the base peak for EDTA in preserved
in water. A molecular weight cutoff of 30,000 Da was chosen to
blood samples, No prominent fragment ions were observed in
remove particulate matter, blood cells, and large proteins from
the spectrum of EDTA, and thus it was necessary to analyze
the filtrate while still maintaining an adequate flow through
samples by LC-M$-MS to obtain structunlly significant ions
the filter disc, A retest by positive ion mode LC-MS-MS of
for identification (Figure 3), In the blood samples, no interseveral dried stains (preserved and unpresennd btood spots)
ferences were found in the reconstructed ion (RIC) tnce for the
produced positive results for all of the EDTA containing blood
MS-MS of ion 293. MS-MS of the 293 ion generated three
with area counts ofseveral hundred thousand for the 160 ion
product ions with a base peak at 160 u and two smaller ions at
and negative results for all unpreserved spots. The sample
that previously had been deemed a negative
(2-trL EDTA blood spot) gave an area count of
Table l. Calculated and Experimenlal tntensity (%) of the Molecular lon
Cluster (CrgHr2N2OsFe) for the lron Complex with EDTA (M - lH+Fettt;1,000,000 for ion 160 by the revised method.'ibo
Observed by Negative lon LC-M$-i4S for an EDTA Standard
of the positive sampies were extnctd a second
time, and it was found that, on average, 9l% of
Predicled
Experimental intensity
the EDTA response (peak area for 160 product
ion) was in the first extract.
342
6,3
6.4
In the negative ion mode, the ferric ion com343
0.8
2.1
plex with EDTAatmlz344, (M
-4H * p.rrl)-, c0n344
f00
t00
sistently appeared in analyses of the disodium
1t,
J{)
EDTA standard and was the base peak for EDTA in
346
2.9
preserved blood samples. The identity of the 344
/.. I
JqI
U.J
ion wu verified by comparing the calculated isou,o
348
U
topic formula for (C1jH12N206Fe) with experi0.2
n/z
intensity
u4b
( szo
mental data (Table I). No prominent structural
Journal of Analy,tical Toxicology, Vol. 21 , November/December I 997
in the LC-MS spectrum of this complex,

MS-MS of the 344 ion gave a strong signal for the product ion
atrnlz 300 (M - C02f. A second LC-MS-MS method, in negative ion mode, was developed to screen for the presence of
EDTA in bloodstains by observing the mass-toclnrge ratio
tnnsition from 344 to 300 in the selected reaction moniiorinf
mode (SRM). This method of MS-MS operation is selective
peaks were observed
10,000
8000
6000
4000
2000
range while measuring a specific trarsition resulting frorn

collision-induced dissociation. The MS-MS ion tnce of rnlz
300 and the RIC show no extnneous signals other than the
major peak for the EDTA derived species from blood extracti
(Figure 6). Some lmown (n = 4) and unknown (n = 2) blood
samples were successfully tested as a trial of the negative ion
method.
A comparison of negative ion and positive ion LC-MS-MS of
a blood stain revealed an 80-fold difference in intensity of
EDTA signal for the 160 ion (positive) over the 300 ion (nega.
tive). Because of [he use of MS-MS in both techniques,
responses from other components in the blood were not
observed, and, therefore, boih analyses were deemed selective
The positive ion mode is a better means of confirmation
because there are three structurally significant product ioru
compared with only one for the negative ion mode.
The IC, negative ion and positive ion LC-MS-MS methods
were used on investigative case samples (n = 9) to determine il
evidentiary crime scene blood might have been tampered evidence. A phenolphtlulein-presumptive test for blood ( 1l ) wa
positive on all testd stains (n = 4). In addition, all extncts of
the stains appeared red in color as supportive evidence for the
praence of blood. All three techniques were negative for EDTA ;
in the bloodstains. Howarer, in the positive ion SRM (mlz tnw a,
sition 293 to 160) LC-MS-MS analysis of one of the stairu.
from a sock, a small peak appeared with the correct retention
time for EDTA" IC and negative ion results did not indicatr
EDIA in the sample and positive ion full scan LC-MS-MS
4.2 0.4
Time (min)
10,000
8000
6000
4000
2000
0
1.2
Fi8ure 6. EDTA analysis of the iron addud ion at ndz344 by negative ion
SRM LC-MtMS. Reconstrucled ion chromatogram (solid line, scan range
297-JO2 u) ard EDTA product ion r/z 100 (dashed line) traces from
unpreservd
and sensitive because the instrument scaru over a limited mass
(A) and tDTA-presewed (B) blood
sain exrfacts.
could not confirm all three EDTA product ions from the parent
ion at 293 u. In known EDTA samples, the three techniques
had consistently agreed, and intersities were strong enough for
ihe known samples to confirm the three product ions by
MS-MS of the parent ion at 293 u. A potential criticism of the
evaluation of the results is the inabilig to determine the exact
quantity of blood in a sample. In these studies, it was found that
sample sizes as small as I pL of blood generated more than adr
quate signal for EDTA. A sample of this size would leave a
dried blood spot of 0.1 cm2 on a swatch of cotton linen.
A study wu conducted to determine if the small unconfirmed signalobserved in the case sample could result froma
carry-over in the system. An EDTA-dt2 standard was used fot
this work to prevent interference from endogenous levelsof
EDTA After sevenlinjections of ttre EDTA-drz standard (500
ppm), blank samples of different substances were run. No
signal by LC-I'IS-MS was observed after a single injection d
blanls such as water, mobile phue, or salt solutions. Howevet,
injection of EDTA free blood extrach, following a blank injec'
tion, gave a response for the EDTA-d12 compound tha[,
decreased with each repetition (Figure 7). The low signal in ti8i
case mentioned above was likely a result of an interferend
resulting from the previously injecterl standard. It is theoiril'
that, when a blank blood matrix is injected onto the s.vstefn,
residualEDTA adsorbed onto sita in the column and hrbintis
released by competing metal ions in the blood extract. There'
fore, it is recommended that the only suitable blank after injr;
tioru of EDTA is EDTA-free blood extncl Multiple injections

EDTA-free blood extract should be made
-1L
/r-: \
ot
uniii no observablqt::,:1,
i#
purnal of Analytical Toxicology, Vol. 21, November/December 1997
EDTA peak is detected before any case samples are anatyzed
this method.
EDTA is an additive in a variety of foods, such as pickla,
canned mushrooms, and salad dresings, and potentially could
occur in human blood at low lewls. However, in a study of
radio-labeled EDTA" ingated samples were found to be eliminated mainly by excretion with minimalgastrointestinal tract
absorption (12). Thus, it is unlikely that measurable quantities
would be found in the blood by the employed techniques,

Attempts to measure EDTA in unpreserved blood by the use of
samples up to I mL in volume were negative. A search of the
literature did not find any measurements of EDTA in blood
from dietary consumption levels.
Another concem in the analysis ofbloodstains is the stability
of EDTA in the dried spots after extended periods of storage.
Samples of EDTA preserved bloodstains (n = 2) were analyzed
after 2 yean of storage at room temperature. LC-MS-MS
analysis of the additive-free samples were negative and the
preserved samples were positive for EDTA"
Conclusion
Methods described herein demonstnte the abili$ to determine if tampering of bloodstains may have occurred using
EDTA-preserved blood The coupling of a quantitative technique with the specificity of the LC-MS-MS procedures is a
powerful analytial protocol. Specific procedures were developed to identifu and control the effect of matrix interference on
0.2 0.4 0.6 0.8
1.2
1.4
Time (min)
the umples. MaFix interference can be minimized by injecting

EDTAlree blood artncts before the analysis of any samples.
The accuracy ofthe determination was supported through the
use of simulated investigative case samples. Experiments on
aged, dried blood indicate it is possible to determine EDTA in
stains after at least 2 years of storage.
Acknowledgments
The authors would like to acknowledge the assistance of
Kelly Hargadon lvtount Jill Smerick, Kathleen Keys, Barban
Koons, Tim Mchughlin, John Paulson, Dean Fetterolf, and
Robert Mothershead, II.
References
1,
2.
0.2 0.4 0.6 0.8
1.2
1.4
nme (min)
Figure 7. Sample carry over experiment to demonstrate the matrix effecl
of blood extracts. The
top chart (A) is an injection of mobile phase after

tire injections of 500 ppm EDTAdl2 standard. The chart on the bottom (8)
shows
the results of injecting an extract from a non-EDTA-preserved

blod tube after the blank analysis in (A). EDTA-d12 analysis of the proton
adducl ion n/z 305
W positive ion iull scan LC-M!MS, Reconstructed
ton chromatogram (solid line) and EDTAdl2 product ion
itne) traces,
r/z
68 (dashed
6.
M. Windholz, Ed. The Merck /ndex. Merck & Co., Rahway, Nl,
'1976, p 463.
,1, De Jon8, A. Van Polanen, and J,J.M. Oriessen. Determination of
ethylenediaminetekaacetic acid and its salts in canned mushrooms by revased-phase ion-pair liquid chromatography. /. Chro
matogt.553i 243-48 (1 991).
C. Retho and L. Diep. Low-level determination of ethylenediaminetetraacetic acid in complex matiices. Z, Lebensm Unters
Forsch. 188: 223-26 (l 989).
B. Nowack, F.C. Kari, S.U. Hilger, and L.Sigg. Determination o{
dissolved and adsorbed EDTA species in water and sediments by
HPLC, Anal. Chen. 68:561-66 (1 996).
P.J.M. Eergers and A.C. De Croot. The analysis of EDTA in water
by HPLC, Wat Res.28:639-42 (1994).
M. Unger, E. Mainka, and W, Konig. Quantitative determination
of EDTA and its behavior in radioactive waste solutions using
HPLC. Fresenius J. Anal. Chem.329: 50-54 (1 987).
4L/b
Journal of Analytical Toxicology, Vol. 21, November/Decemhr
E,L.
Inhan, R.L. Clemens, and I'A. Olsen. Determination of
EDTA in vancomycin by liquid chromatography with absorbance

AnaL S (6):
ratioing for peak identification. J. Pharm.
513-20 (1990).
BioM.
8.
'10.
Hamilton application note #286,287.

P. Kebarle and L. Tang. From ions in solution to ions in the gas
ohase, Anal. Chern. 55(22)1 9724-86A (1 993).
C.f. tjames, R.C Dutky, and H.M. Fales. lron carboxylate oxygentriangle complexes detected during electrospray use of organic
acid modifien with a comment on the Finnigan TSQ'70 elec'
trospray inlet system. /. Arn. Soc. Mass Spec, 5: I 226-31 (l 995).
1997
ll,
W,C. Eckert and S.H. lames. lnterytetation of Blodstain Evi.

dence at Crime Scenes. CRC Press, Ann Arbor, Ml, 1993, p 120.
12. H. Foreman and T.T. Trujillo. The metabolism of raC labeld
ethylenediaminetetraacetic acid in human beings, /, Lab. Clin,
Med.43;566-71 (1954).
Manuscript received January 31, 1997;

revision received Aoril 29, 1997.
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AC
8197:
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Determining EDTA in Blood
I of6
Analytical ChemistrY
August l, L997
Analytical Chemistry 1991,69, 477 A-480L'
Copyright @ lggi by the American Chemical Society'

b
Amurdertrialshedslightontheneedforabetteranalyticalmethod
Robjn-,L-,-$he-p,pard
JaskH-enion
Cornell UniversitY
news uses words such as "liquid chromatography" and
It is not often that a story on the national evening
,,mass spectrometry'i"Ai"iyti";l chemists who lieard such reports.during the murder tnalrhe state of
perked up their ears, amazed that the analytical
carifurnia v. orentharT"riiiii^pson immediately
headlines'
J.tuits of FBI laboratory testing were actually making
(ethylenediaminetetraacetic acid) issue was whether police had

The subject of the testing was EDTA
,,planted,, or tampereJ *Ttn Utooa evidencl in an attempt to shore up the case against Simpson' The
i"Jirg were simple: Either EbTA-was present or it wasn't. Qualitative testing
possibre outcomes
"r,r,.
is that simple. There was eYidence of some EDTA, at levels
began (i), but as is usually the iase, l:lfrllg
The questions "How much EDTA is there?" and "Are the
much lower than in;DTi-;r"served bloodl
in
with'normal' levels or those that would result from tainted blood collected
detected levels
"orrririrnt
blood tubes?" arose immediately.
E iA anticoagulant
to present this scientific evidence. But how do you
The lead prosecutor, Marcia Clark, tried her best
about analytical chemistry that the EDTA came not from a
convince a jury or.itir.", that knows little
o.J. Simpson? Althoug! i!.mav not have been the only
lavender-stoppered lrrt. u,rt from a bleeding
*ur u factor in the trial's outcome. Because of this
weak point in the prosecution's case, it certiinly
has become a topic of renewed interest'
criminal case, determining EDTA in human blood
it was not clear whether the method had ever been

what was wrong with the laboratory testing? First,
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Page 2 of 6
AC8197 Determining EDTA in Blood
the method was developed quickly under a great deal of time pressure. In
carryover in the
,etrorpe"t, FBI chemisti now believe that the EDTA detected may have been injection
run before the
had
been
blank
a
matrix
of
lCnfSnrnS (2) instrumentation because a water blank instead
volume
of the
Se.oni, the EDTA concentration was not rigorously quantitated, Cert-ainly, the
(-1300 ppm) in EDTAblood stain could have been estimated. EDTA is present at about 4.5 mM
by electrospray
detected
easily
preserued blood, which would be a very concentrated sample and
blood samples was orders of
LC1MS/I\4S. It appeared that the amount of EDTA detected in the forensic
became apparent that a
magnltuae below 4.5 mM. Regardless of what happened in the Simpson trial, it
and valid method foi determining EDTA in human blood was needed.
used before. Most
likely
*-pf.
definitive
EDTA I}ASTCS
in the early 1950s
EDTA is a metal-complexing agent that has been popular since its commercialization
a threeand
weight of 292.1 is shown in Figure 1a,
i-rj. rr* free-acid structure *itrr u molecular
weight of 347.0 is
dimensional representation of EDTA complexed with nickel(Il) with a molecular
solution pH values of
at
ionized
sequentially
are
shown in Figure lb. EDTA has four acidii protons t!{
as
an anticoagulant (5)'
used
2I,2.67,6.i6, and lo.z6,respectively ({. The disodium salt is commonly
enough EDTA to give a final
and the familiar lavender-stoppered biood collection tubes contain
chelates the available
immediately
EDTA
the
blood,
concentration of - 4.5 mM. Uion mixing with
cannot take place (5).
coagulation
calcium. Because calcium is necessary for the formation of fibrin,
trl
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il
W-s
dor
,*S*
oru&z'4't{O-i-*
tDl
structure of Ni-EDTA'
Figure 1. (a) EDTA's free-acid structure and (b) three-dimensional
and to deliver trace

EDTA is also used extensively as a food preservative, a water-softening agent,
have shown that little,
studies
metabolism
minerals in animal feeds (e. bespite its ubiquitous presence,
laco-lubel.d
if any, EDTA should be present in human blood. In 1954, a metabolism study using
plasma but not in the
calcium-EDTA given intravenously showed that EDTA was detectable in the
and feces within three days
blood cells ( Z). 6r, u,u"rug e, 95o/o of an oral dose was recovered in the urine
was detected in the urine
57o
remaining
of administration with no EDTA detected in the plasma, and the
within 1g h. More recent metabolism studies using the NaFe(III)-EDTA complex report that it
is absorbed and excreted in
dissociates during digestion and confirm that only about 5% of the EDTA
urine (8).
DETERMINING EDTA IN BLOOD AND PLASMA

EDTA in various matrices such as
Although there are numerous published methods fo).a.t"t-ining
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AC
8197:
Page 3
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mayonnaise (9), wastewater (/0), and ophthalmic solutions (11), our lab and one other group have
reclntly attempied to develop improved methods that could be used for the forensic measurement of
EDTA in biological matrices (12, 13).
There are numerous ways to prepare samples containing free or chelated EDTA. The first and most
obvious is no sample pieparation at all. If the pH of the sample is not adjusted and if metal
contamination can be eliminated, the natural distribution of EDTA and its metal chelates can be
determined. This is not the most sensitive approach because the EDTA signal would be distributed
among several different metal species or peaks. In addition,.quantitation would be difficult because any
to
chang-e in the sample matrix could change the complex equilibria. Therefore, all the methods used
peak
or
compound.
EDTA-containing
a
singular
preparing
*""r-ur" EDTA itielf focus on
For GC, the analyte must be reasonably volatile and thermally stable. Because EDTA is not volatile, it is
usually derivatized by esterifying the four carboxyl groups with methanol, butanol, or isopropyl aicohol
(13-l i). This liquid-iiquid extraction is a labor-intensive, multistep procedure that is difficult to
automate. For L-C or capillary electrophoresis (CE), the most logical way to convert all available EDTA
to a single compound is to aOA an exCess of one metal that strongly complexes with EDTA. Although
iron(Illj and copper(Il) are commonly used (,11, 16),we found that nickel(Il) complexes with EDTA just
anA iihas several advantages: Heating is not required, the complex is stable down to
u.
"if.rtiu"ty,
pH\t3, and the complex gives a higher signal by ion spray MS than either the iron or copper complexes.
DEVELOPING A CE/MS/MS METHOD

Several reports in which CE was used to determine metals using EDTA as a.complexing reagent have
predicted that an
been published in the literature (17, /8). Using these reports as a starting point, we
additives introduced
the
chemical
"MS-hendly" CE separation could be developed that would minimize
into the mass sPectrometer.
The intricacy of interfacing the capillary to a mass spectrometer is the reason the technique is considered
nonroutine. Although many qualitative CEA{S applications have been reported, very few quantitative
methods have been described in the literature (19,20). Therefore, we used this opportunity to achieve
two goals: to offer an improved technique for measuring E-DTA in biological matrices and to
deminstrate that CE/MS can be used in a routine manner for quantitative bioanalytical applications.
Although MS may not be the most sensitive CE detector available, it offers a high level of selectivity as
well asaider appiicability than, for example, laser-induced fluorescence (21). For example, the full-scan
different metal complexes.
CEI11{S separation shown in Figure 2a displays the EDTA dishibuted as five
Figure 2b shows the same EDTA standard in which the predominant ion m/2347, caused by Ni-EDTA,
ha! been extracted from the total ion current data. This type of selectivity can be exploited by using the
selected ion monitoring mode in which only the ion(s) of interest would be detected.
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AC 8/97: Determining EDTA in Blood
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(b) extracted ion electropherogram

Figure 2. (a) Full-scan GE/IVIS electropherogram of five EDTA-metal chelates and
of Ni-EDTA.
that is characteristic of
Additional selectivity can be achieved using MS/TvIS by selecting a precursor ion
on specific fragment from
the analyte, fragmenling it into one or more ions, and selectively detecting
the Ni-EDTA complex in
the selected prJcurso. i6n. For example, a full-scan single mass spectrum of
the [Ni2+"H+
Figure 3a shows the deprotonated molecular anion at m/z 347, which corresponds to
,gbre4-]- ion. This precursor ion may be fragmented using collision-ind1cgd dissociation within the
product ion mass
.econd-quadrupole region of a triple-quadrupole mass spectrometer. The full-scan
m/z 347-inFigure 3b shows product ions m/z 329 and 257, which
;;;il; from the fralmentation-ofcomplex'
are characteristic of the Ni-EDTA
tsf
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o
t87
tm
i4t {lt
,so
nt
of Ni-EDTA'
Figure 3. (a) Fult-scan mass spectrum and (b) full-scan product ion scan
mode by
This additional selectivity can be put to use in the selected reaction m-onitoring ISnfuO
is achieved via
to
3.29.l"t*:=fctivity
monitoring only the rpr.ifi.d traniition m/z 347 fragmenting
It
is
highly unlikely
Ni-EDTA.
the initial LE separation, which gives a characteristic migration time for
characteristic transition at the
that a chemical compound otherihan Ni-EDTA would result in this
conditions'
specifred migration iime under the described experimental
simply diluted with water'

To illustrate this point, blank and Ni-EDTA-spiked p!a9m1 samples were
The blank plasma in
detection.
and analyzed 6y CE with tIV detection and CE with SRM
filtered,'4a
because
andthe t-pvrNi-EDTA-spiked plasma in Figure_4b are indistinguishable by CE/W
Figur.
ofrn. excessive chemical background detected at200 nm. In contrast, when analyzed by SRM-CE^VIS'
(Figure 4c); whereas the Ni-EDTA-spiked
the same blank plasma sample i-s free of all matrix peaks
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AC 8197 Determining EDTA in Blood
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plasma displays only the targeted Ni-EDTA peak (Figure 4d). This example clearly shows the advantage
of using tandem MS for this type of targeted analysis.
tr)
t3
t'l-r
't
Ifto Frrif
243
rrulnul
aat
rfmF{6}
?46
frhlt!|il
Figure 4. UV detection versus SRM detection.
CEruV analysis of (a) blank plasma and (b) Ni-EDTA-spiked plasma. SRM-CEA4S analysis from m/z 347 to 329 of (c)
blank plasma and (d) Ni-EDTA-spiked plasma.
To further minimize the possibility of interference, we developed an automated anion-exchange solidphase extraction procedure. The complete SRM-CEA4S procedure uses 100 pL of plasma, to which is
added 50 ng of 113C0;EDTA internal standard, brought to pH 9-10 with ammonium hydroxide, and
complexed using nickel nitrate. The sample is diluted 1:45 with 0.05% formic acid (pH 3) and then
extracted using itrong anion-exchange solid-phase extraction media. The sample is eluted, evaporated,
and reconstituied in 30 pL of water. The extract is injected for 0.1 min at 950 mbar inlet pressure onto a
50 pm X 60 crn amine-coated capillary. The separation is performed using a CE running buffer of 30
*M u--onium formate atpH 3 (adjusted with formic acid) and -30 kV with 50-mbar inlet pressure
throughout the run. A homemade self-aligning liquid junction CEA4S interface is used with a makeup
liquiJof 5 mM ammonium formate in95o/o methanol at lOpl/min(22,23). Atriple-quadrupole mass
splctrometer is used in the negative-ion mode with SRM of the transitions m/z 347-329 for Ni-EDTA
and m/z 35 1-333 for the internal standard Ni-(13C4)EDTA. The complete method and validation are
described
in this issue in reference24,
Using this sample preparation procedure and the SRM-CE/\4S method, we achieved a detection limit of
(-6 frnol
7.3 n:glmL EDiA in human plasma and a lower level of quantitation (LLQ) of 15 ng/ml
iniecled). If this method waJused to determine whether a forensic blood stain had been "planted", this
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AC
8197: Determining
Page 6
EDTA in Blood
of6
LLQ conesponds to "planting" 1-3 nL of EDTA-preserved blood. Because it would be physically

difficult to manipulate such a small volume, any such forensic sample would probably contain at least I
pL. This hypothetical scenario illustrates the excellent sensitivity and potential forensic usefulness of the
method. Similarly, the GCilvIS/I4S method developed by Ballard and colleagues demonstrated a
comparable detection limit of 10 ng/sample, which corresponds to -7 or 8 nL of EDTA-preserved blood
(13).
CONCLT-ISIONS
Many techniques have been used over the years to determine EDTA in various matrices, and most can
be adapted to biological samples. Howevet, SRM-CEA4S provides the highest specificity and the best
detection level of any method currently published.
.
We have been able to demonstrate that typical human plasma samples do contain detectable EDTA, but
at levels that are lower than the LLQ reported in this work. The LLQ of our method, at 15 ng/ml, is a
factor of 105 lower than the typical concentration found in EDTA-preserved blood (4.5 mM or 1.3 X 106
ng/ml.). But more importantly, we have demonstrated that CE/lvIS methods can be used for routine
bioanalytical analysis with acceptable precision, accuracy, and adequate detection levels for quantitation
of trace-level concentrations (24).
CE/MS techniques will undoubtedly become an important forensic technique because of the low
volumes of sample required for analysis, as well as the ability to use the mass spectrometer to achieve
selectivity higher than with any other on-line detector.
The question of blood-evidence tampering in a oriminal trial has led not only to improved analytical
techniques for the determination of EDTA, but also to the demonstration that a relatively new technique
is ready to be used as credible scientific evidence in the courtroom.
REFERENCES
tF
ChemCent"t
Pubs Div. I'lome Page
Copyright @ 1997 by the American Chemical Society.
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Insrumert Opcrattoo g SunniLs2:.b;:

Issue Date: 0621/06
l:;lfl;3
Performance Monitoring Protocol (QA/QC)
for the Finnigan LCQ LClMS @Sf)
1
Scope
This document addresses the performance monitoring (QA/QC) of the Finnigan LCQ LC/MS
to
system consisting of a Finnigan LCQ MS and a Waters LC. It is an analytical instrument used
its
11nalyzea wide u*i.ty of evidence and must be maintained in such away as to verify
reproducibility from analysis to analysis and its reliability in court.
2 Principle
LCe system is comprised of a Waters Liquid Cluomatograph (LC) and a Finnigan ion trap
LCe Mass Spectrometei (VfS). The instrument is configured with an API source that is capable
The
of Uotn electrospray (ESI) and atnospheric pressure chemical (APCI) ionization.
The
for APCI
instrument is primariiy used in ESI mode. However, this protocol can also be used
provided the method of ionization is clearly labeled in the resulting data and documentation.
befinitions and guidelines for following this protocol are outlined in the "General lnstrument
Maintenance PolicY."
3 EquipmenUMaterials/Reagents
a.
lnstrumentation - Finnigan LCQ MS, API Source, Waters Alliance 269012695 LC,
and Data System with XCalibur software (or equivalent)
b.
API Gas - Nitrogen, 99.99% (high purity or equivalent)
c.
Ion Trap Gas - Helium,99.99yo (high purity or equivalent)
d.
Methanol, HPLC grade

Deionized Water, 18 M(.l Milli-Q or equivalent
Acetonitrile, HPLC grade

g
Acetic Acid, reagent grade
44b
( s;.,i]1
r,:*lfff#
Insrumurt Operation & Support.Subunit
l:;:tr3
h.
Ulftamark 1621 (Finnigan or equivalent)
i.
Caffeine (Sigrna or equivalent)
j.
MRFA (L-methionyl-arginyl-phenylalanyl-alanine acetate) (Finnigan or equivalent)
k.
Ammonium Hydroxide (NruOD, reagent grcde
l.
Codeine (Sigma or equivalent)
m.
Brucine (Sigma or equivalent)
n.
Reserpine (Sigma or equivalent)
o.
Volumetric glassware
p.
Infusion Syringe
10 to 500 pL LC syringe (Hamilton or equivalent)

4.1 Testmix
The Testrnix is used to assess daily operating performance, mass assignment, and continued
integrity of the system. To prepare, weigh 5.0 mg caffeine, 1.0 mg codeine, 1.0 mg brucine, and
1.0 mg reserpine into a 100-mL volumetric flask. Bring to the mark with methanol and mix well.
Store the solution in the refrigerator. It has a shelf-life of three years. This preparation may be
appropriately scaled up.
4.2 Cahbrttion Solution

The calibration solution is used for coarse tuning and calibrating the mass spectrometer over the
entire mass range. This procedure only needs to be performed when the instrument has been
moved, down for a long period of time, undergone a major repair, or warranted based on system
performance.
The calibration solution is a solution of caffeine, MRFA, and Ulhamark 1621 in
acetonitrile:methanol:water containing l% acetic acid. To prepare this solution, follow the
procedure in the LCQ 'Getting Started' manual. Store the solution in the refrigerator. It has a
shelf-life of three years. This preparation may be appropriately scaled up.
fn
q*,( s+")
FBI Laboraory
Chemistry Unit
Insrument Operation & Support Subunit

Inst 202-0.doc
Issue Date: 06nl/06
Revision: 0
Pase 3 of 8
5 Calibration
The calibration procedure should be performed as needed, when the instrument has been moved,
down for a long period of time, undergone a major repair, or warranted based on system
performance.
a.
Load a 250 pL syringe with the calibration solution.
b.
Using capillary tubing, connect the infusion syringe to the ESI probe assembly, and
place in the syringe pump.
c.
Set the syringe pump to the correct syringe type and set the pump rate
tol0
pl/minute.
d.
Load the tune file "ESI TLTNE" (or equivalent).
e.
Check that instrument is in POSITIVE ION mode and collecting CENTROID data.
f.
Set the detector using the parameters listed in the 'Instrumental Conditions' section
of
this protocol.
g.
Turn on the syringe pump and verifu that the solution is flowing out the ESI needle.
h.
Engage the ESI probe and turn on the MS.
i.
In Tune Plus, open the Calibrate dialog box, choose the'Automatic'tab and check the
individual tests or'Select All' and then 'Start.'
j.
When the calibration is complete, it

successful.
o
.
k.
will display
whether or not the calibration was
If
the procedure fails, repeat the calibration.

When the procedure passes, print the report and evaluate the calibration
solution spectrum using the 'Decision Criteria' section of this protocol. If the
results are acceptable, print the spectrum of the calibration solution.
If all requirements
are within specification, prepnre the documentation as outlined
the "General Instrument Maintenance
Policy." If any requirements fail, the IOSS
This is an uncontrolled copy of a controlled documenl
/4{.
( sr)
in
H:#ltr"f#
Insu,ment Operatt"" U r
"*:to!:oblill
lil:'lr3
Manager
will
determine the corrective action to be taken.
6 Sampling
Not applicable.
7 Procedures
7.1 Daily Checks
The following steps are to be performed
log for tracking purposes.
a.
daily. Enter the appropriate information in the QA/QC
Record the remaining disk space on the hard drive. Use Windows Explorer program
(WindowsNT) to verify that the hard disk has at least 100 MB of free disk space. Do
not use if less than 100 MB remain.
b,
Record the line pressure of the building nifrogen supply (API gas). The regulator
should read between 60 and 100 p.s.i. If it cannot maintain this pressure, contact
IOSS. If the nitrogen'is supplied by a gas cylinder, record the tank pressure. change
c.
Record the line pressure of the building helium supply (ion trap gas). The regulator
should read between 30 and 60 p.s.i. If it cannot maintain this pressure, contact
Ioss. If the helium is supplied by a gas cylinder, record the tank pressure. change
d.
Check the Ion Gauge to ensure that no significant leaks are present in the system. Do
not use if the pressure is higher than I x 10* torr.
Prepare the instrument for analysis of Testnix. Verify that the instrument has the
conect source probe installed (ESI), the correct tune file loaded (esi_tune or
equivalent), positive ion mode selected, and centroid data being collected. If a
column is installed, remove it from that system and replace it with the infusion
capillary tube.
Perform an analysis of the Testnix prior to the analysis of evidence using parameters
listed in the'Instrumental Conditions'section of this protocol. Start the HPLC pump.
Engage the ESI probe and turn on the MS. Start an acquisition using a filename such
O,g"
(sqi
FBI Laboraiory
rnstnrment operati""
rififf Hff ll
Inst 202-0.doc
Issue Date:
06nll06
lilii:i3
equivalent). Make three 5 pL injections of the Testnix solution
approximately 10 seconds apart by using the manual loop injector, and then stop the
data collection. Evaluate the results using the 'Decision Criteria' section of this
protocol. If the results are acceptable, print the TIC and spectra for all components in
as 'testmix' (or
the Tesrnix.
g.
If all requirements
within specification, prepare the documentation as outlined in

the "General lnstrument Maintenance Policy." If any requirements fail, contact
are
IOSS.
7.2 As Needed Checks
a.
Re-cut or replace the sample capillary as needed.
b.
Clean or replace the heated capillary as needed.
Refer to the "General Instument Maintenance Policy" for procedures on minor deviations.
8.1 Testmix
Liquid Chromatoeraph
Mobile Phase:
Flow Rate:
Column:
lnj Volume:
Number of Inj:
95:5 methanol:water + 0.03% ammonium hydroxide

0.2
ml/min
None
5pL
a
Mass Spectrometer
Ionization:
Tune File:
Scan Mode:
Scan Range:
ESI
esi_tune
Full Scan
100-650 miz
C-
4(6
(s /')
FBI Laboratory
Chemistry Unit
Insrument Operation & Support Subunit
Inst 2024.doc
Issue Date: 06nl/06
Revision: 0
page 6 of 8
8.2 Calibration
Mass Spectrometer
Ionization:
ESI
Tune File:
esi_tune
Scan Mode:
Scan Range:
Full Scan
100-2000 mlz
9 Decision Criteria
9.1 Testmix
Verify the results of the Tesftnix. The following ions should be observed in the three Testrnix
injections:
. Caffeine I95 mlz
. Codeine 300 mlz
o Brucine 395 mlz
r Reserpine 609 mlz
9.2 Calibration
Veri$
the results of the calibration. The calibration will indicate

successful. The individual ions for the calibration solution are:
r
r
r
Caffeine
L95 mlz
MRFA
524 mlz
Ultramark 1022m/z
Il22
mlz
L222mJz
1322m/z
mlz
1422
1522
1622
1722
1822
L922
m/z
mlz
mlz
mlz
mlz
if
the procedure was
greater than 5%
greater than 50%
greater than 5o/o
greater than2DYo
greater than 50%
greater than 50%
greater than 80%
greater than 50%
greater than 50%
greater 'han 20o/o
greater than l0%o
present
Eo q,/,
(sv+)
FBI laboratory
Instrument operatt""
& s:lof,t'HbYJ l:
Inst 202-0.doc
Revision: 0
Page 7 of 8
10 Calculations
Not applicable.
Not applicable.
12 Limitations
Only properly trained personnel shall perform duties involved in the operation, maintenance, or
troubleshooting of this instrument.
13 Safety
Take standard precautions for the handling of all chemicals, reagents, and standards. Refer to
the FBI Laboratory Sof"ty Manual for the proper handling and disposal of all chemicals.
Personal protective equipment should be used when handling any chemical and when performing
any t)?e of analysis. Many instrument components are held at temperatures of 250oC and
higher. Precautions should be taken to prevent the contact of skin with heated surfaces and
areas.
14 References
Manufacturer's lnsfument Manuals for the specific models and accessories used.
"General Instrument Maintenance Policy" (Inst 001) Instrument Operation and Support Subunit
SOP Manual.
"Liquid Chromatograph General Maintenance Protocol" (Inst 003) Instrument Operation and
"Mass Spectrometer General Maintenance Protocol" (Inst 004) Instrument Operation and
FBI Laboratory Safety Manual.
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Memo
To:
tr'rom:
Date:
Subject:
Madeline A. Montgohory, Marc A. LeBeau

Cynthia L. Morris-Kukoski
February 26,2007
Competency EDTA
uL
Madeline Montgomery successfully completed her competency test for the EDTA in
Bloodstains SOP. She 100% correctly identified which blood samples contained EDTA and
which ones did not.
Q,t+e,
(
uot)
competnrcytest
Date:
212012007
To:
LEBEAU, MARC A. (LD) (FBD
From:
Jay A.
RE:
Competency Test
Clark ,5['
Congratulations, you have successfully completed your competency exam for the Analysis of EDTA
in Blood Stains.
Please see the attached Key for the correct answers, and the procedure for the preparation of the test
samnles.
v'/4u
(u"4
competnrcytestkey
Date:
211512007
RE:
Competency Test Key
Competency Tests for Analysis of EDTA in Blood Stains results are as follows
JCI
non-preserved blood
JC2
EDTA preserved blood
JC3 - EDTA preserved blood

JC4 - EDTA preserved blood
JQJ:- norypreserved blood

JC6'- EDTA preserved blood
.':
JC7
noir:preserved blood
t:
:cB
JC9
t n*-Pteserved blood
- EDTA preserved blood
:l''"rl
ldt0 -
non-preserved blood
Prepared
Date:
Yy,
(htT.}la'h--
1-
t5-07
fn qqL
(t *)
Preparation of Competency Tests for "Analysis of EDTA in Blood Stains" SOP:
1.
Seiect a sterile cotton-tip swab and label
Z.
Place
3.
Repeat
4,
Allow all swabs to dry overnight. Blindly distibute to test participants.
it with a unique identifier.
onto the cotton

EDTA.
containing
tip swab. Document if the swab was prepared with blood
l0 pL of blood @DTA-preserved or non-EDTA-preserved)

with appropriate number of swabs.
f"
'-tqr-
( u'4
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Datez 2/2812007
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99-18A
413012002 11:59:59PM
Staff Position SUPERVISORY CHEMIST-UNIT CHIEF

Test
Complete Examination & Analysis
Most Recent Proficiensy Test
QualificaUons Date
Identifier
iIFi ffr]TKl
Quantitative - Drug Analysis
Toxicology
tlLlI999
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QualTypeLinklD
000000000000275
CAP
Preparer Name
Extemal
Verifier Name
Chemistry Unit
Validator Name
Other Comments
LT-mM Noufication of Test 5/1/2000 12:00:00AM
Distribution Date
LIlLlt999
Due Date
L2lL6lL999 12:00:00AM
PT Complete Date
l2ltllL999
Testee
Feedback
rntifier
5/3/2000
12:00:00AM
12:00:00AM
12:00:00AM
Supplier
00-17
-rff Position SUPERVISORY CHEMIST-UNIT CHIEF

Test
Source
LD-PTPM Eval
College of American PathologisE
Preparer Name
Verifier Name
Extemal
Validator Name
Source Unit
Other Comments
LT-mM Noufication of Test
Distribution Date
ltlL6l2000
Due Date
L2lZLl2000 11:59:59PM
LD-FI?M Review Notified
PT Complete Date
1212612000 12:00:00AM
Testee Feedback
5/712001 12:00:00AM
LD.MM
Identifier
12:00;00AM
Source
Unit
EVaI
Supplier
01-15

Test Source Extemal
51217001 12:00:00AM
CAP
Preparer Name
Verifier Name
Validator Name
Chemistry Unit
Other Comments
Distribution Date
8lL3l200L 12:00:00AM
LT-ffiM
Due Date
91251200L 12:00:00AM
LD-mM Review
PT Complete Date
91251200L 12:00:00AM
UC Desisnee Final
Testee Feedback
t2l3t/200t
LD-PTPM Eval
12:00:00AM
IdenUfier 02-2
'rce Unit
NoUfication of
Test
Notified
Supplier
Eval
12731/2001 12:00:00AM
LZl3tlZ}}L
12:00:00AM
1213112001 12:00:00AM
College of American Pathologists
Preparer Name
Verifier Name
Validator Name
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CqtG
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Setailed Qua$ifications and Froficiency Test

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217812007
qeport Description:
to view detailed
Detailed Qualifications and Profrciency Test Report for MARC A LEBEAU 0781-0000
of Test
31L812002 12;00:00AM
Due Date
413012002 11:59:59PM
PT Complete Date
413012002 12:00:00AM
Testee Feedback
71L612002 12:00:00AM
LD.PTPM EvaI
Identifier
Supplier
03-27A

Source Unit
71L612002 12:00:00AM
Preparer Name
Verifier Name
Validator Name
Other Comments See attached memos
Test 1/15/2004
Distribution Date
L012712003 12:00:00AM
LT-PTPM NoUfi cation of
Due Date
LLl712003 11:59:59PM
LD.PTPM Review NoUfied
PT Complete Date
t2l9lZ003 12:00:00AM
Testee Feedback
L012004 12:00:00AM
LD-PTPM Eval
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12:00:00AM
Setalled Qualifications and F

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212812007
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iTU Personnel use this
lo view detailed
Detailed Qualifications and Proficiency Test Report for MARC A LEBEAU 0731-0000
Toxicology
Qualifications Date
L/t/L999
QualitaUve
- Drug Analysis
Interprebuon of Results
12:00:00AM
Identifier
PT
519/2007 11:59:5BPM
Supplier
05-58
Staff Position
Verifier Name
Source Unlt
Validator Name
College of American PathologisE
Preparer Name
Other Comments FTC-A- satisfactory compleUon
Date
Date
PT Complete Date
Testee Feedback
Distribution
3fl7lzOOS 12:00:00AM
Due
SfinOOS 11:59:59pM
SF?OOS 12;00;00AM
Bl5l2OOS t2:00:00AM
LD-PTPM Eval
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Supplier
06-38
-aff Position
Verifier Name
Source Unit
Validator Name
Test 5/5/2005
12:00:00AM
Preparer Name
Other Comments
Distribution Date
3/t612006 12:00:00AM
Due Date
sl8l2oo5 11:59:59PM
LD-FIPM Review Notified
PT Complete Date
Testee Feedback
513/2006 i2:00:00AM
12:00:0OAM
Test 5/3/2006
LD-PTPM Eval
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Page ,. of 1
12:00:00AM
QuaffypeLinklD
000000000000738
nralificatiosrs and FrofEclency Test Report
Setailed
Date;
212812007
R.eport Description:
to view detailed ualifications and
Qualibative - Drug Analysis
Toxicology
12:00:00AM
Identifier
Supplier
994
Source
Source
Unit
PT
Lt/512004 11:59:59PM
413012002 11:59:59PM

Test
Qualifications Date
LltlL999
Complete Examination &,Analysis
Qual[ypeLinklD
000000000000274
CAP
Preparer Name
External
Verifier Name
Chemistry Unit
Validator Name
Other CommenE
LT-mM Notificauon of feC(. 31L711999 12:00:00AM
Distribution Date
3lL7/t999
Due Date
31291t999 12;00:00AM
LD-PIPM Review
PT Complete Date
71211999 12:00:00AM
UC Desisnee
Testee Feedback
81411999 12:00:00AM
LD-PTPM Eval
'entifier
Unit
Notifled 7lt3lt999
FinalEval
CHEMIST-UNIT CHIEF
12:00:00AM
8/10/1999 12:00:00AM
3/15i2000 12:00:00AM
Supplier
00-6
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Test Source Elternal
Source
12:00:00AM
CAP
Preparer Name
Verifler Name
Valldator Name
Chemistry Unit
Other Comments
Distribution Date
61712000 12:00:00AM
Due Date
61t912000 12:00:00AM
LD-PTPM Review
PT Complete Date
6ltgl2010
Uc Deslgnee Final
Testee Feedback
Identifier
12;00:00AM
8/30/2000 12:00:00AM
Test
Source
Source
Unit
Eval
12:00:00AM
8/30/2000 12:00:00AM
812912000 12:00:00AM
LD.PTPM EVaI
Supplier
01-15
Test 8/30/2000
Notified
CAP
Preoarer Name
External
Verifier Name
Chemistry Unit
Validator Name
Other Comments
Distribution Date
Due Date
PT Complete Date
Testee Feedback
IdenUfier
8/13/2001 12:00:00AM
9125/?00t 12:00:00AM
9lZ5l200L 12:00:00AM
L2/3U200L 12:00:00AM
02-24
Staff Position SUPERVIS0RY CHEMIST-UNIT CHIEF
Test
Source
'''Jrce
External
Unit
LD-PTPM Review
UC Desisnee
Test
Notified
FinalEval
1213U2001 12;00:00AM
Lzl3tl200t
12:00:00AM
1213112001 12:00:00AM
LD-PTPM Eval
Supplier
Preparer Name
Verifler Name
Validator Name
-rher Comments
5o
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*ate:,
212812007
'eport Description:
to view detailed qualifications and
Detailed Qualifications and Proficiency Test Report for MARC A LEBEAU 0731-0000
DistribuUon
3lt9l2002
Due Date
413012002 11:59:59PM
LT-ffiM
LD-ffiM
PT Complete Date
4/3012002 12:00:00AM
Testee Feedback
71t612002 12:00:00AM
LD-PTPM Eval
Identifier
12:00:00AM
Notification of
Supplier
03-27A

Verifier Name
Source Unit
Validator Name
Other Commenb
Distribution Date
7lt6lZ002 12:00:00AM
Review NoUfied
Preparer Name
See attached memos

LT-PTPM Notifi cation of
Test 1/15/2004
t012712003 12:00:00AM
LLl712003 11:59:59PM
PT Complete Date
LZl9l2003 12:00:00AM
Testee Feedback
2/1012004 12:00:00AM
LD-PTPM Eval
Due Date
/ /,
Cv Vlb
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( utal
Fnoe 2 nf 2
12:00:00AM
S-etailed Quallfications and Froflclenr

Date:
T'est Repoft
2128120Q7
Repoff Descriptionl
to view detailed oualifications and
Toxicology
Qualifications Date
Interpretation of Resulb
Blood Alcohol
Expiration Date wlthout a new
L/t12004 12:00:00AM
IdenUfier
91212007 11:59:58PM
Supplier
05-27A
Source
External
Comments
College of American PathologisB
Verifier Name
CAP AL1-C- satisfactory completion
Test
Distribution Date
10i5l2005 12:00:00AM
Due Date
L012012005 t1:59:59PM
LD-F|PM Review Notified
PT Complete Date
t011412005 12:00:00AM
L21t212005 12:00:00AM
Testee Feedback
'rntifier
Source
10/1412005 12:00:00AM
LD-PTPM EVaI
Supplier
06-14A
,ff Position
Test
000000000000736
Validator Name
Source Unit
Other
QuaflypeLinklD
Preparer Name
Staff Position
Test
PT
Preparer Name
Verifier Name
External
Validator Name
Source Unit
Other Comments
Distribution Date
61t912006 12:00:00AM
Due Date
613012006 11:59:59PM
LT-PTPM Notification of Test

PT Complete Date
Testee Feedback
LD.PTPM EvaI
Identifier
Supplier
06-13A
Test
Source
Quality Forenics
Preparer Name
Staff Position
Verifier Name
External
Validator Name
Source Unit
Other Comments
Telr. 7FI:Z006
Distribution Date
712112006 12:00:00AM
LT-PrPM Notification of
Due Date
91t12006 11:59:59PM
LD-PTPM Review Notifled
712112006 12:00:00AM
PT
Complete Date
Testee Feedback
LD-PTPM EVaI
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VVb
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Paqe L df
12:00:00AM
Setailed
Date:
ualificaticns and
Test
2lZBIZOOT
Q.eport Descriptionl
to.Jlgw detailed ualifications

and
Lest for selected staff.

Detailed euafifications
proficiency
and
Test Report for MARC A
LEBEAU 0731-0000
@
Toxicology
Blood Alcohol
Qualifications Date
t/t/L999
12;00:00AM
Identifier
9g-7
Unit
Expiration Date witfrout

a new
L0/20/2004 12:00;00AM
Staff PosiUon SUPERVISORY

CHEMIST_UNIT CHIEF
Source
Complete Examination &

Analysis
Most Recent proficiency Test
Chemistry Unit
pT
L0/20/20C4 11:S9:S9PM
Supplier
QualTypeLinklD
000000000000272
CAp
Preparer Name
Verifier Name
Validator Name
Other Comments
Distribution Date
6/1511999 12:00:00AM
6/2s11999 12:00:00AM
6/2211999 12:00:00AM
Due Date
PT Complete Date
Testee Feedback
'ntifier
,ff
8/4/1999 12;00:00AM
00-12
Position SUPERVISORY CHEMIST-UNIT
LT-PTPM NoUfi cation of

Test
LD.PTPM Eval
Supplier
CHIEF
Source Unit
6/15/1999 12;00:00AM
6/24/1999 12:00;00AM
8/10/1999 12:00:00AM
3/15/2000 12:00:00AM
Preparer Name
Verifler Name
Validator Name
Other Commenb
Distribution Date
9/1912000 12;00:0OAM
9/2912000 11:59:59pM
9/2912000 12;00:00AM
Due Date
PT Complete Date
Testee Feedback
L2/18/2000 12:00:00AM
IdenUfier
01-164
Staff Position SUPERVISORY
CHEMIST.UNIT CHIEF
Test Source
External
Source Unit
Chemistry Unit
Test
LD-PIPM Review Notified
t2/4/2000 12;00:00AM
LD-PTPM Eval
Supplier
CAp
Preparer Name
Verifier Name
Validator Name
Other Comments
Distribution Date
Due Date
PT Complete Date
Testee Feedback
9/t81200t 12:00:0oAM
9/27/200t 12:00:0OAM
9/241200t 12:00:0OAM
2/18/2002 12:00:0OAM
Identifier
02-188
Staff Position SUPERVISORY
CHEMIST-UNTT CHIEF
Test Source
External
,rce Unit
vLner Comments
LT.PTPM Nouficauon of
Test
LD-PTPM Eval
Supplier
Preparer Name
Verifier Name
Validator Name
5o,
(a
2/18/2002 12:00:0oAM
2/18/2002 12:00:0OAM
2t6t2002 12:00:00AM
College of American pathologis8
iletailed Quallfications and Fnofic

Date:
T'est Re
212812007
teport Description;
to view detailed
Detailed Qualifications and Proficiency Test Report for MAR.C A LEBEAU 0731-0000
Distribution Date
t0lt9l2002
Due Date
t0/2512002 11:59:58PM
12:00:00PM
LT-ffiM
Notification of
PT Complete Date
1012512002 11:00:00AM
Testee Feedback
tU26/2002 12:00:00AM
LD-PTPM EvaI
Identifier
Supplier
03-25A
1012512002 11:00:00AM

Verifier Name
Source Unit
Validator Name
College of American pathologisb
PreDarer Name
Other Comments
Distribution Date
10/15/2003 12:00:00AM
Due Date
PT Complete Date
t012812003 11:59:59PM
1012t12003 12:00:00AM
Testee Feedback
Lt/24/2003 12:00:00AM
LD-PTPM Eval
Test t0/2112003
{* u+e,
( o,)
Paqe 2 of ?
12:00:00AM
Setailed Qerafrlfications asld Ps's$iclency Test Repoft

*ate:
212812007
Repo* Descrlptionl
to view detailed
test for selected staff,
and
Detailed Qualifications and Proficiency Test R.eport for MARC A LEBEAU 0731-0000
Drug Analysis
Qualifications Date
L/r/t999
Identifier
Source
Source
12:00:00AM
Unit
QualTypeLinkID
000000000000224
Supplier
99-5A

Test
Complete ExaminaUon & Analysis
CTS
Preparer Name
Extemal
Verifier Name
Chemistry Unlt
Validator Name
Other Comments
Distribution Date
5/18/1999 12;00:00AM
LT-PTPM Notification oF Test
7lL3lL999 12:00:00AM
Due Date
7181t999 12:00:00AM
PT Complete Date
7lUL999 12:00:00AM
ilt31t999 12:00:00AM
8/10/1999 12:00:00AM
Testee Feedback
8141t999 12r00:00AM
LD-PTPM Eval
3/15/2000 12100:00AM
':ntifier
Supplier
00-38
"aff Position SUPERVISORY CHEMIST-UNIT CHIEF

Source
Unit
Chemistry Unit
CTS
Preparer Name
Verifier Name
Validator Name
Other Comments
Distribution Date
51312000 12:00:00AM
LT-PTPM NoUfi cation of Test
81712000 12:00:00AM
Due Date
612812000 12:00:00AM
8/712000 12:00:00AM
PT Complete Date
611312000 12:00:00AM
712812000 12:00:00AM
Testee Feedback
817/2000 12:00:00AM
LD-PTPM Eval
{o qqu
(
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Page 1 a{
Detalled Qwalificatiosrs and F

*atet
2/2812007
{epoft Sescription;
legt for selected staff.
iletailed Qualifications and Froficienry Test Report for MARC A LE8EAU 0yBt-000O
Trace Analysis (Chem,)
Bank Dyes
Qualifications Date
LltlL999
Most Recent Profi ciency Test
Identifier
Source
Source
Expiration Date wi$rout a new
12:00:00AM
Unit
pT
t21612002 11:59:59pM
99-38
QualTypeLinklD
000000000000261
Supplier

Test
Preparer
Name
Internal
Verifier Name
Chemistry Unit
Validator Name
Waninger, Eileen Marie
Oher Comments
Distribution Date
3lt6lL999
Due Date
41271t999 12:00:00AM
LD-PTPM Review
4/t91L999 12:00:00AM
UC Designee Finat
41271L999 12;00:00AM
LD-PTPM
PT
Complete Date
Testee Feedback
12:00:00AM
LT-PTPM Notifi cauon of
Eval
TeSt
Notified
Evat
1999 12:00:00AM
Sn7/Lggg 12:00:00AM
5/4/1ggg 12:00:00AM
31IS/ZOOO 12:00:00AM
&,/qa,
r'r,l)
Page
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of
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Setailed Quallfications aEld Froficlemcy Test Report
*ate;
212812007
?eport ilescription:
to view detalled
ifications and
Detailed Qualifications and Froficiency Tast Repont for MADELINE A MONTGOMER.Y 07It-0S00
Quantibtive - Drug Analysis
Toxicology
QualifioUons Date
LlIlL999
12:00:00AM
Identifier
QuaftypeLinklD
L2lL6lt999 12;00;00AM
512512002 1l:59:SBPM
000000000000275
Supplier
99-18A
Staff Position CHEMIST-FORENSIC EGMINER

Test
Source
Source
Unit
CAP
Preparer Name
External
Verifier Name
Chemistry Unit
Validator Name
Other Comments
Distribution Date
PT Complete Date
LllLl1999 12:00:00AM
LZlt6lL999 12:00:00AM
tZlL0lL999 12:00:00AM
Testee Feedback
51212000 12:00:00AM
LD-PTPM Eval
Due Date
.ntifier
,ff Position
Test Source
00-17
Supplier
CHEMIST-FORENSIC EGMINER
Preparer Name
External
Verifier Name
Source Unit
Test 5/1/2000 12:00:00AM
LD-PTPM Review Notlfled
Validator Name
Other Comments
TeSt
Distribution Date
ILl612000 12:00:00AM
Due Date
t2/21/2000 11:59:59PM
PT Complete Date
1212612000 12:00:00AM
Testee Feedback
5l14/2001 12:00:00AM
LD-PTPM Eval
Identifier
Supplier
01-3
stAff Position CHEMIST.FORENSIC EKAMINER

Test
Source
Source
Unit
5/7 12001 12:00:00AM
CAP
Preparer Name
External
Verifier Name
Chemistry Unit
Validator Name
Other Comments
Distribution Date
3lL6l200L 12:00:00AM
6/5/2041 12:00:00AM
Due Date
412612001 12;00:00AM
6151200t 12:00:00AM
PT Complete Date
41201200L 12:00:00AM
61412001 12:00:00AM
Testee Feedback
614/200t 12:00:00AM
LD-PTPM Eval
Identifier 02-4
Staff Position CHEMIST-FORENSIC E0MINER
'rce Unit
Supplier
Preparer Name
Verifier Name
Validator Name
vtner comments
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Setal$ed
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[!_fg1so-nnel use this report to view detailed qualifications and
Detailed Qualifications and Froficiency Test Report for MADELINE A Mor.{TGOMERY 0731-0000
Date
Date
PT Complete Date
Testee Feedback
Distribution
Due
312S1ZOOZ !Z:OO:O
11:59:59pM
12:00:00AM
LL14/ZOOI 12:00:O0AM
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to view detailed
Oetailed Qualifications and Proficiency Test Report for IvIADELINE A MONTGOMERY 0791-0000
Quantitative - Drug Analysis
Toxicology
Qualifications Date
Most Recent Proficienry Test
QualTypeLinkID
7/t12002 12:00:00AM
511412003 11:59:59PM
L211712007 11:59:58PM
000000000000276
Identlfier
Supplier
02-12A
Staff Position CHEMIST-FORENSIC EXAMINER

Verifier Name
Source Unit
Validator Name
PreDarer Name
Other Comments
Distribution Date
7/2/2002 12:00:00AM
LT-mM
Due Date
7lt5l2002
LD-FTPM Review Notified
PT Complete Date
7/9/2002 12:00:00AM
Testee Feedback
ItlL5l2002
LD.PTPM EVaI
11:59:59PM
12:00:00AM
'ntifier
NoUflcation of
Supplier
03-4A
Position
CHEMIST-FORENSIC
EXAMINER
-.aff
Test Source Extemal
Verifier Name
Source Unit
Validator Name
Test 8/16/2002
12:00:00AM
Preparer Name
Other Comments
fegr
Distribution Date
312612003 12;00:00AM
LT-mM
Due Date
511412003 11:59:59PM
PT Complete Date
4/25/2003 12:00:00AM
Testee Feedback
712912003 12:00:00AM
LD-PTPM Eval
Identifier
NotificaUon of
Supplier
04-20A
StAff Position CHEMIST.FORENSIC ENMINER
Preparer Name
Verifier Name
Source Unit
Validator Name
4/ZS1Z003 12:00:00AM
Quality Forenics
Other Comments
Distribution Date
L0/2612004 12:00:00AM
LT-my
Due Date
1211612004 12:00:00AM
PT Complete Date
LL/9/2004 12:00:00AM
Notificauon of
Testee Feedback
LD-PTPM Eval
Identifier
Supplier
05-238
Staff Position
rrce Unit
Test 1/18/2005
Quality Forenics
Preparer Name
Verifier Name
Validator Name
other Comments
UY/\ VVb
(bao1
12:00:00AM
Setnlled
aate:
uallfications amd Fs'oficierucy ?est Re
212812007
oeport Description:
Oetailed Qualifications and Proficiency Test Report for MADE!-trNE A MONTGOMERY 073t.-0S00
Ltl712005 12:00:00AM
LT-PTPM
Due Date
t21L612005 11:59:59PM
PT Complete Date
L211412005 12:00:00AM
Testee Feedback
121t412006 12:00:00AM
LD-PTPM Eval
Identifier
Supplier
06-34
Staff Position
Test
t21L412005 12:00:00AM
Preoarer Name
Source E*ernal
Verifier Name
Validator Name
Source Unit
Other Comments
Distribution Date
312212046 12:00:00AM
LT-PTPM NoUfi cauon of T
Due Date
5/812006 11:59:59PM
LD-FIPM Review NoUfied
PT Complete Date
411312006 12:00:00AM
Testee Feedback
16i2006 12:00:00AM
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LD-PTPM Eval
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Faqe 2 of 2
4I
L3 12006 12:00:00AM
;:{
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2128120Q7
Report Description:
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Detailed Qualifications and Froficiency Test Report for MADELINE A MONTGOMERY 0Ig1-0000
ryryWW
Toxicology
dws.'I {:1 a KTJTFI n
Qualitative
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71t12002 12:00:00AM
5/14/2003 11:59:59PM
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PT
L211512007 11:59:58PM
Position CHEMIST-FORENSIC EXAMINER
Preparer Name
Test
Source
Verifier Name
External
StafF
Source Unit
Supplier
02-12A
III
Analysis
Qualifications Date
IdenUfier
ff*l ff-;K
QualTypeLinklD
000000000000274
College of American Pafrologists
Validator Name
Other Comments
Test 8/16/2002
Distribution Date
712/2002 12:00:00AM
Due Date
711512002 11:59:59PM
PT Complete Date
7/9/2007 12:00:00AM
Testee Feedback
Ltlt5l2002
LD-PTPM Eval
rnUfier
12:00:00AM
Supplier
03-4A
.rff Position CHEMIST-FORENSIC EXAMINER

Test
Source
External
12:
00:00AM
Preparer Name
Verifier Name
Source Unit
Validator Name
Other Comments
Distribution Date
312612003 12:00:00AM
LT-ffiM
Due Date
51L412003 11:59:59PM
LD-PFPM Review Notified
PT Complete Date
4/2512003 12:00:00AM
Testee Feedback
712912003 12:00:00AM
LD-PTPM EVaI
Identifier
Notifi cation ot
Supplier
04-204
Staff Position CHEMIST-FORENSIC EKAMINER

Verifier Name
Source Unit
Validator Name
Test 4 l2S/2003
12:00:00AM
Quality Forenics
Preparer Name
Other Comments
Test 1/19/2005
Distribution Date
1012612004 12:00:00AM
Due Date
PT Complete Date
L2/t612004 12:00:00AM
LUgl2A04 12:00:00AM
Testee Feedback
Ll1812005 12:00:00AM
LD-PTPM Eval
Identifier
05-238
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'rrce Unit
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LIl712005 12:00:00AM
LZlL4l2005 11:59:59PM
LT-FIPM NotiflcaUon of Test
PT Complete Date
L211412005 12:00:00AM
Testee Feedback
L211412006 12:00:00AM
LD-PTPM Eval
Due Date
Identifier
06-3A
L21L412005 12:00:00AM
Supplier
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Test Source E*ernal
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Other Comments
Distribution Date
312212006 12:00:00AM
LT-PTPM NoUfication of Test
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51812006 11:59:59PM
LD-P|PM Review Notifled
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41t312006 12:00:00AM
Testee Feedback
16/2006 12:00:00AM
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Unit
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Chemistry Unit
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Sample Prep,,Wet Chem. & Inst. Analysis
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Identifier
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CAP
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Validator Name
Other Comments
Distribution Date
3lL7/1999 12:00:00AM
3lL7/1999 12:00:00AM
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312911999 12:00:00AM
7lI3lL999
PT Complete Date
7121t999 12:00:00AM
8141t999 12:00:00AM
8/10/1999 12:00:00AM
LD-PTPM Eval
31t512000 12:00:00AM
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Source
Source
Unit
12:00:00AM
CAP
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External
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Validator Name
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61712000 12:00:00AM
Due Date
6/t912000 12:00:00AM
LD-ffPM Review Notified
8/30/2000 12:00:00AM
PT Complete Date
611912000 12:00:00AM
812912000 12:00:00AM
Testee Feedback
8/30/2000 12:00:00AM
LD-PTPM Eval
Identifier
Supplier
01-3

Test
Source
Source
Unit
LT-FIPM NoUfication of Test 8/30/2000 12:00:00AM
CAP
Preparer Name
Extemal
Verifler Name
Chemistry Unit
Validator Name
Other Comments
Distrlbution Date
3/16/200t 12:00:00AM
LT-PTPM NoUfi cation of Test
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312912001 12:00:00AM
LD-ffPM Review Noufied
6/51200L 12:00:00AM
3/281200t 12:00:00AM
61412001 12:00:00AM
6/4/200t
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Testee Feedback
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02-4
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Detailed Qualifications and Proficiency Test Report for MADELINE A MoNTGoMERy

0731-0000
Date
Date
DistribuUon
3/25/200t
Due
5/2412002
Date
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PT complete
12
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Toxicology
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Source Llnit
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Distribution Date
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Due Date
71712003 11;59:59PM
LD-FIPM Review NoUfied
PT Complete Date
7/t12003 12:00:00AM
Testee Feedback
712912003 12:00:00AM
LD-PTPM Eval
Identifler 04-2A
Verifier Name
Source Unit
Validator Name
Supplier
TesI
7/
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2003 12:00:00AM
Preoarer Name
Other Comments
Date
Date
PT Complete Date
Testee Feedback
Distribution
3D12OO4 12:00:00AM
LT-P|PM Notification of
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3123/2004 11:59:59pM
3fl7lZOO4 12:00:00AM
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3lfil1111 1Z:00:00AM
7ltBlZ}lS 12:00:00AM
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12:00:00AM
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Testee Feedback
Distribution
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rzlLlzoo6 11:59:59pM
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4.epott Descripticn:
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CIetailed Qualification$ and Proficiency Test Report for MADELINE A MONTGOMER.Y 0731-0S00
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8141t999 12:00:00AM
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Notified
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612411999 t2:00:00AM
8/10/1999 12:00:00AM
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LD-PTPM Eval
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00-12
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CAP
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LD-PTPM Eval
Identifier
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Test
Source
Source
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12118/2000 12:00:00AM
tzltBlZ000 12:00:00AM
121412000 12:00:00AM
CAP
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Testee Feedback
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t2t2001 12:00:00AM
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212812007
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tTU Personnel use this
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Oetailed Qualifications and Frcficiency Test Report for MADELINE A MOr-|TGOMERY 0731-0000
Drug Analysis
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911012003 11;59:59PM
Identifier
Source
External
PT
912312007 l1:59:58PM
Supplier
03-12A

Test

QuatTypeLinklD
000000000000224
Preparer Name
Verifier Name
Source Unit
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Other Comments
Distribution Date
7/30/2003 12:00:00AM
Due Date
911012003 11:59:59PM
PT Complete Date
B/13/2003 12:00:00AM
Testee Feedback
L2/212003 12:00:00AM
LD-PTPM Eval
'ntifier
.rff Position
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Source
04-13A
Supplier
CHEMIST-FORENSIC EXAMINER
Preparer Name
External
Verifier Name
Source Unit
Test 8/13/2003 t2:00:00AM
Validator Name
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Test 10/2612004
Distribution Date
7/L512004 12:00:00AM
Due Date
Bl26l20M 11:59:59PM
PT Complete Date
L0/2612004 12:00:00AM
Testee Feedback
1012612004 12:00:00AM
LD-PTPM Eval
Identifier
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05-15A
Staff Position
Test
Source
Extemal
Verifier Name
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Comments
CTS 05-502- saUsfactory completion
Date
Due Date
PT Complete Date
Testee Feedback
Distribution
Identifier
CollaboraUve Testing Services
Preparer Name
Source Unit
Other
12:00r00AM
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Date:
2/2812007
qeport Description:
Detailed Qualifications and Froficiency Test Report for MADELINE A MoNTsoMER.y 0731-0000
Distribution Date
3/2212006 12:00:00AM
Due Date
51812006 11:59:59PM
Notification of T
LD-ffiM
Review Notified
PT Complete Date
Testee Feedback
LD-PTPM Eval
Identifier
Supplier
06-174
Staff Position
Test Source Extemal
Verifier Name
Source Unit
Validator Name
Preparer Name
Other CommenE
Distribution Date
8/10/2006 12;00:00AM
Due Date
912212005 11:59:59PM
LD-ffiM
PT Complete Date
91t412006 12:00:00AM
12/412006 12:00:00AM
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12:00:00AM
Identifier
Source
QualificaUons Date
Test
III
Drug Analysis
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EI i 4rtrFl n rrfr I ir'IEn
CIS
Preparer Name
External
Verifier Name
Chemistry Unit
Validator Name
Other Comments
DistribuUon Date
L0ltl1999
Due Date
tLlL9lt999
PT Complete Date
Testee Feedback
rntifier
12:00:00AM
Unit
NoUfi
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212912000 12:00:00AM
2l29l2OOO 12:00:00AM
LLl4lL999 12:00r00AM
212812000 12:00:00AM
212912000 12:00:00AM
LD-PTPM Eval
3/15/2000 12:00:00AM
Supplier
00- 11C
-dff Position CHEMIST-FORENSIC EOMINER

Source
LT-ffPM
12:00:00AM
ChemisW Unit
CTS
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Distribution Date
813112000 12:00:00AM
LT-P|PM Noufication of Test
L2lLBl2000 12:00:00AM
Due Date
10/30/20oo 12:00:00AM
10/16/2000 12:00:00AM
L?/L8t2000 12;00:00AM
L211812000 12:00:00AM
1211812000 12:00:00AM
PT Complete Date
Testee Feedback
LD-PTPM EVaI
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Setalled
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2/2812007
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test for selected stafi.
Detailed Qualifications and Proficiency Test Report for EILEEN MARIE WANINGER 0731-00S0
Drug Analysis
Qualifications Date
L/t/1999
Source
Source
Unit
PT
912312007 11:59:58PM
Supplier
99-5E

Test
ExpiraUon Date without a new
Iol8l2o04 12:00:0bAM
12:00:00AM
Identifier

QualTypeLinKD
000000000000224
CTS
Preparer Name
External
Verifier Name
Chemistry Unit
Validator Name
Other Comments
Distribution Date
5l18/1999 12:00:00AM
7lB/L999 12:00:00AM
7ll3lt999
7/131t999 12:00:00AM
PT Complete Date
61291t999 12:00:00AM
8/10/1999 12:00:00AM
Testee Feedback
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LD-PTPM Eval
31t512000 12:00:00AM
Due Date
ntifier
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00-3D
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Test Source E*ernal

Source
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Cfs
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LT-F|PM NoUfication of Test 8/7/2000 12:00:00AM

LD-PfPM Review NoUfied
8/712000 12:00:00AM
PT Complete Date
612012000 12:00:00AM
Testee Feedback
8/7/2000 12:00:00AM
LD-PTPM Eval
Identifier
01-5A
Source
Unit
Chemistry Unit
Supplier
712812000 12:00:00AM
CTS
Preparer Name
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Distribution Date
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LT-PTPM NoUfication of Test
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PT Complete Date
4lt0l200L
611112001 12:00:00AM
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02-lC

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LD-PTPM Eval
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Detailed Qssalificatloffis and Fnoflciemcy Test R.epoft

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esl
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Testee Feedback
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LD-PTPM Eval
Identifier
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03-1D

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| 112002 12:00:00AM
Preparer Name
Verifier Name
External
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Source Unit
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UC Designee Flnal Eval
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Identifier
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Supplier
Staff iosition
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121212003 12:00:00AM
Testee Feedback
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Re-Examination
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Source Unit
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LD-PTPM Eval
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10/2612004 12:00:00AM
CTS 05-502-saUsfactory completion
B/10/2005 12:00:00AM
LT-ffPM Notification of TesI 812412005 12:00:00AM
912212005 11:59:59PM
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Detailed Qualifications and Prcflciency Test R.epcrt for EILEEN MAruE WAHINSER 0731-0000
Identifier 06-17C
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Staff
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External
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Test
Source
CollaboraUve Testing Services
Verifier Name
Validator Name
Other Comments
Date
Date
rr complete Date
Testee Feedback
12:00:00AM
11:59:59PM
91712006 12:00:00AM
121412006 12:00:00AM
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8ln?006
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912212006
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Setailed Qualifications and Proficiency Test Report for EILEEI{ MARIE WANINGER 0731-00S0
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Trace Analysis (Chem.)
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L012312003 11:59:59PM
Identifier
99-3F
Source Internal
Source
Unit
812L12007 11;59:59PM
PT
Quafl'ypeLinklD
000000000000261
Supplier

Test
Preparer
Name
Wang, Deborah
Verifier Name
Chemistry Unit
Validator Name
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3/t61L999 12:00:00AM
LT-FrPM Noufication of
Due Date
41271t999 12:00:00AM
LD-PTPM Review
PT Complete Date
3/261L999 12:00:00AM
UC Designee Final
Testee Feedback
41271L999 l2:00:00AM
LD-PTPM Eval
DistribuUon Date
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:]5I 5lL7lL999 12:00:00AM
Notified
Eval
SlL7lL999 12:00:00AM
51411999 12:00:00AM
3/1s/2000 12:00:00AM
Supplier
00-8C
-.aff Position CHEMIST-FORENSIC E$MINER

Test Source internal
Source Unit Chemistry Unit
Preparer
Name
Cook, Pamela
C.
Verifier Name
Validator Name
Ofier Commenb Test 00-B was withdrawn and a new test was reissued.
Distribution Date
711012000 12:00:00AM
Due Date
Bl2Il2O00 12:00:00AM

PT Complete Date
Testee Feedback
LD-PTPM Eval
Identifier
Supplier
00-14D
Staff Position CHEMIST-FORENSIC E$MINER

Test
Source Internal
Source
Unit
Preparer
Name
Cook, Pamela
C.
Verifier Name
Validator Name
Chemistry Unit
Other Comments
Test
12118/2000 r2:00:00AM
NoUfled
!2/1812000 12:00:00AM
Distribution Date
9/2612000 12:00:00AM
LT-FrPM Notification of
Due Date
Ltl9l2000
LD-PTPM Review
PT Complete Date
912812000 12:00:00AM
UC Desisnee
Testee Feedback
LZlt9l2000 12:00:00AM
LD-PTPM Eval
Identifier
12:00:00AM
01-11C
Staff Position CHEN4IST-FORENSIC EXAMINER

Test
Source Intemal
rce
Unit
Chemistry Unit
FinalEval
1211812000 12:00:00AM
Supplier
Preparer
Name
Wang, Deborah
Verifier Name
Validator Name
Other Comments
fo uvt
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Setai[ed
X$ficatias, s
and Pogftgtency Test Report
&ate: Zl2el2007
ceport Description:
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test for selected staff,
Detailed Qualificaticns and Proficiency Test Report for EILEEN MARIE WANINGER 0731-0000
bution Date
71L912001. 12:00:00AM
Due Date
912512001 12:00:00AM
91251200t 12:00:00AM
PT Complete Date
8/3012007 12:00:00AM
7/3112001 12:00:00AM
Testee Feedback
912512001 12:00:00AM
91251200t 12;00:00AM
LD-PTPM Eval
Identifier
02-168
Test Source Intemal
Source
Unit
D7-LABORATORY DIVISION
Supplier
Preparer
Name
Name
Verifier
Validator
Name
DEBOMH WANG
MICHAEL P RICKENBACH
DEBOMH WANG
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DistribuUon Date
9/2612002 5:00:00PM
LT-PrPM Noufication
Due Date
ttl8l2002
LD-ffPM Review NoUfied
12:00:00AM
ofTest 10/2512002
PT Complete Date
L0/24/2002 12:00;00PM
Iestee Feedback
t2l9/2002 12:00:00AM
LD-PTPM Eval
Identifler
03-13C
9:00:00AM
Supplier

Verifier
SourceUnit
Validator
D7-CHEMISTRY
Preparer
Name
Name
Name
DEBOMH WANG
MICHAEL p RICKENBACH
DEBOMH WANG
er Comments
Distribution Date
9lLLl2003 12:00:00AM
LT-PTPM NotlficaUon of
Due Date
LO/2312003 11:59:59PM
PT Complete Date
101312003 12:00:00AM
Testee Feedback
L0/2712003 12:00:00AM
LD-PTPM Eval
Identifter
04-BC
Unit
12:00:00AM
Supplier
Staff Position CHEMIST-FORENSIC EOMINER

Test Source Intemal
Source
Test 10/3/2003
CU
Preparer
Verifier
Name
Name
Validator
Name
DEBOMH WANG
ROBERT F MOTHERSHEAD
DEBOMH WANG
Other Comments
Distribution Date
6/23/2004 12:00:00AM
8/412004 11:59:59PM
LT-PTPM Notjfication of
PT Complete Date
613012004 12:00:00AM
Testee Feedback
6/30/2004 12:00:00AM
LD-PTPM Eval
Due Date
Identifier
05-10C
Unit
Distribution Date
n're Date
:omplete Date
r
Preparer
estee Feedback
Name
VerifierName
Validator Name
CHEMISTRY
Other Comments
12:00:00AM
Supplier
Staff Position
Source
TesI 6n012004
TEST SET
DEBOMH WANG
ROBERTMOTHERSHEAD
DEBORAH WANG
#1- satisfactory compleuon
Test 5/19/2005
5/18/2005 12:00:00AM
6129/2005 11:59;59PM
5/1812005 12:00:00AM

8lLLl2005 12:00:00AM
LD-PTPM Eval
&,/,1,
b)t
12:00:00AM
Setalled Qura$$ficatiosls and Froficiency Test Report

sate:
2/2812007
oeport Sescription:
.\TU Personnel use this
to view detailed
Detailed Qualifications and Proficiency Test Report for EILEEN MARIE WANINGER 0731-0000
Identifier 06-258
Supplier
Position
Source Unit Chemistry
Staff
Preparer
Verifier
Name
Name
Validator
Name
Pamela Reynolds
Eileen Waninger
Jason Brewer
Other Comments
Date
Date
PT Compfete Date
Testee Feedback
12:00:00AM
11:59:59PM
512612006 12:00100AM
6lL'lz006 12:00:00AM
ofTest 5/2612006
Distribution
5/18/2006
LT-PTPM Nouflcation
Due
613012006
LD-PTPM Review Noufied

LD-FTPM Eval
4(6
(asl
Pase 3
of3
12:00:00AM

Trial Exhibit 446 EDTA Lab Sheets and Reports

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Trial Exhibit 446 EDTA Lab Sheets and Reports

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U.S.

Federal Bureau of Investigation

Washington, D. C 20s3 5-000

February 28, 2007

Calumet County District

RE: State of Wisconsin v. Steven Averv

I am wrJ-ting in response to a letter f rom rlerome F.

{^r 4'l l(i )

"l\ny and all valiclation studies the FBI has done.

Enclosed is a copy of the validation studies.

Information regarding studies referred to in the

st,udies referred to in...,,

Information regarding studies referred t.o in t.he

"Any complaints or negative performance evaluations. . .,,

Pursuant to IIBI Policy, a review of t,he Examiner,s

"Instrument run 1og with identification of aII. . . "

"Records of instrr.rment maintenance status and..."

Enclosed is er copy of the maintenance records of

"An error or contamination 1og covering any and a1l..."

contamination that occurred in other cases is bevond

data f or the complete measurement sequence. . . ,,

A11 information regarding the raw data for this

r hope this materi.al will assist vou in this effort.

lfit tL. .//lI

50-rh D:doF *flBrt anl NyN - f Tfr

Atl<6p {btA_ 6 BLI-T- StuPL (, o/u.) nr) oa/

ct't\ ou1 ?\W

(tou - Frt+ DLe-*-zs,v

f uAct-p r^J L,t'Be c cp

BTANK (neg blood, Dl H2O ext.)

ESI SRM ms2

ESI SRM ns2

ESI SRM ms2

ESI SRM ms2

BIANK (neg blood, Dl HZO ext.)

BLANK (neg blood, Dl H2O ext.)

ESI SRM ms2

r/z= 325.S326.5 Fi. c

BLANK (neg blood, Dl H2O ext.)

BLANK (neg blood, Dl H2O ext.)

Card C extract (EDTA +)

ESI SR[,] ms2

ESI SRM ms2

BLANK (neg blood, Dl H2O

ESI sRM ns2

BLANK (neg blood, Dl H2O ext.)

Card D extract (EDTA

ESI SRM ms2

BIANK (neg blood, Dl H2O ext.)

ESI SRM ms2

ESI SRM msz

ESI SRM ms2

BLANK (neg blood, Dl H2O ext.)

ESI SRU ms2

ESI SRM ms2

BLANK (neg blood, Dl H2O ext.)

ESI SRM ms2

BIANK (neg blood, Dl H2O ext)

ESI SRM ms2

Card F extract (EDTA +)

ESI SRM mE2

BLANK (neg blood, Dl H2O ext.)

ESI SRM ms2

BI-ANK (neg blood, Dl H2O ext.)