A Test for Evaluation of the Serum Separation Potential of

Tomato Ketchup
NIKOLAOS G. STOFOROS and DAVID S. REID

ABSTRACT MATERIALS & METHODS

The tendency of tomato ketchup to separate into a structural solids Ketchup sample preparation
phase and a serum phase was measuredby placing a small amount of A typical homogenizedcommercial ketchup (McCormick and Com-
ketchup on a wire screen mounted at the bottom of a plexiglass tube. pany Inc., Hunt Valley, MD) was used. The effect of storage tem-
The screen retained structural solids along with bound serum while perature on serum separationwas then studied using nonhomogenizcd
unbound serum drained through and collected in a holder tube ketchup samples prepared from 32 Brix concentrate tomato paste.
below the screen. Rate and degree of separation were particularly The paste was obtained from tomatoes of the UC 204 variety using
applicable to study separation potential of single serving ketchup conventional Hot Break or Cold Break procedures. Batches of
pouches. Although reducing storage temperature decreasedinitial rate 200-1OOOgketchup were prepared using the method described by
of serum separation, final amount of serum loss was independent of Marsh et al. (1979a). Details of the procedure, starting from raw
temperature. tomatoes and ending with ketchup, are reported elsewhere (Stoforos,
1984).
INTRODUCTION
AMONG THE PROPERTIESof ketchupthat determineits Serum separation test
gradeis the tendencyof the productto retainthe liquid portion For serum separation measurements, a screen tube was con-
in suspension(Anon, 1953).Phaseseparationin tomatoket- structed by the Food Science and Technology Department shop. A
chupis particularlyapparent in someindividualservingpouches stainless steel screen (60 mesh/inch, wire size 0.190 mm, openings
but testsprovidelittle informationconcerningserumseparation 0.234 mm) was mounted at one end of a 2.54 cm outside diameter
potentialof ketchup.Factorsdeterminingthe qualityof tomato pIexiglass tube as shown in Fig. 1. A 50 mL polypropylene centrifuge
productsin termsof consistencyhavebeenidentified.How- tube (Nalgene #3110-9500) was used to hold the screen tube.
ever, thin or thick ketchupsmay haveeithera high or At the beginning of each test, the weights of holder tube, and the
screen tube and holder tube combined were measured (~0.1 mg).
low degreeof serumseparation(Davis et al., 1954; Twigg, The combined tubes were placed into a test tube rack and, using a
1959;Marshet al., 1979b;Shomeret al., 1983).In the blotter plastic pipet, S-5.5 g ketchup samples were carefully applied on the
test a ketchupsampleis appliedto a filter paperand the dis- screen. Care was taken to not force the sample through the screen and
tanceof serumflow on the paper,measuredafter an appro- to ensure that the sample was forming an even, slightly domed shape
priatetime, is usedasanindicatorof separation potential(Nelson on the screen without extending up the sidewalls of the screen tube.
et al., 1957).Twigg (1959),comparingthe blotter test with
the rate of filtration test (filtration undervacuumof diluted
sample,McCollahet al., 1950)selectedthe blotter as more
appropriatefor serumseparation measurements.However,Palma
(1983)showedthe resultsobtainedusingthe blotter testwere
dependenton the rate of evaporationof water from the filter
paper,thatis, uponthe humiditysurrounding theblotter.Also,
he found no relationshipbetweenserumflow on the blotter
and separationof ketchupin individualservingpouches.An-
other serumseparationindicatoris a new type of Bostwick
consistometer which measuresdistancebetweenthe point of
colorlessliquid and the red body in a given period of time
(Gould, 1983).Resultsfrom a gravity sedimentation test (Ro-
binsonet al., 1956; Smit and Nortje, 1958)were also corre-
lated with tendencyof serumfor separation(Shomeret al.,
1983).Serumseparationin tomatojuice was also measured
by Caradecet al. (1985)by monitoringthe amountof serum
drainedthrougha 60cone-shaped 42 meshscreen.
However,in singleportionketchuppacks,individualpouches
can have very different degreesof separation,even though
filled from the same,presumablyuniform, sub-batchof ket-
chup. Thus study of only the bulk propertiesof ketchupis
clearlynot sufficientto understand serumseparation
in pouches.
The effect of variousparameters on serumseparationcannot
be studiedunlessreliablequantitativemeasurements can be
obtained.The purposeof this studywas to developa reliable
test indicativeof the serumseparationpotentialof ketchupin
individualservingpouches.

The authors are affiliated with the Dept. of Food Science &
Technology, Univ. of California, Davis, CA 95616. Fig. 1 -Schematic diagram of the screen tube.

1626-JOURNAL OF FOOD SCIENCE-Volume 55, No. 6, 1990

 headspaceduring sealing. The orientation of the pouchesduring stor-
age affected both the air bubble position and the slope of the ketchup
surface which was in contact with the air bubble. Serum separation
40 was affected by these factors.
3
0A30
Gravity sedimentation test
I
z Ketchup We,ght (g, A gravity sedimentation test was also performed and correlation
820 -a- 2.64 betweenthis test and the serum separationpotential was tested. During
s -o- 5.22 the gravity sedimentation test, one part ketchup was diluted with six
-v- 8.42 parts (by weight) water or the artificial strum previously described.
10
-o- 11.58 The samples were allowed to settle at least 1 month in 18x50 mm
-D- 17.40
rimless culture tubes covered with parafilm. During this time, the
P/L ratio versus time was calculatedby measuringthe solids precipiate
0'. II I, I- I, II I, I- I II I
100 200 300 400 500 600 700 800 900 1000
height (P) and the total height (L) of the sample. The 1:7 dilution was
0
used to obtain acceleratedseparation, since at lower dilutions many
TIME (hours) homogenizedketchup samplesshow little separationin the time scale
Fig. Z-Effect of ketchup sample weight on serum separation. of the experiment.
Each point represents the average of three replicates while each
bar indicates one standard deviation. RESULTS & DISCUSSION
Determining optimum sample mass
Table 1 -Coefficients associated with Eq. (1) for the experiments with Preliminaryexperiments were performedto determinethe
different ketchup sample weight
preferred samplemassto be usedduringserumseparation tests.
Ketchup A
weight (g)' (hr) B R2
Differentweightsof homogenized commercialketchupsam-
2.64-cO.10 0.0600 0.0372 0.989
plesweretested.Theresultsof percentserumlossversustim e
5.22kO.09 0.1471 0.0282 0.987 are presented in F ig. 2. The asymptotictrendof the percent
8.42eO.09 0.2625 0.0267 0.983 serumloss versustim e curveswas also observedin all sub-
11.58*0.17 0.3416 0.0302 0.957 sequentexperiments on serumseparation[about80 different
17.40t0.39 0.6166 0.0344 0.964 experimental conditions(Stoforos,1984)].A regression equa-
a Average of three replicates f one standard deviation tion foundto adequately predictpercentserumlossas a func-
tion of time, in all cases,was
No attempts to change the shape of the sample were made. In case
of unevenly delivered sample, the test was redone. The weight of the SL = t
A+Bt (1)
combined tubeswith the ketchup samplewas obtainedat the beginning
and the end of each test in order to determine the sample weight and wheret represents the elapsedtim e in hours,andA (hour)and
to ensure that no weight loss occurred during the experiment. To
prevent evaporation, the tubes with the ketchup sample were placed B (dimensionless) aree m p iricalconstants.FromEq. (l), tak-
in a desiccator containing about 3.5 cm artificial serum in the ing the lim it as tim e approaches infinity, we found that l/B
bottom. The artificial serum was preparedusing the same method as represents the final percent serum loss. By differentiating Eq.
that for ketchup preparation (Stoforos, 1984), but with high fructose (1) with respectto tim e andtakingthe lim it of the resulting
corn sweetener(42 Be) substituted for tomato paste to result in the expression astim e goesto zero,l/A canbe shownto represent
same soluble solids content as the ketchup samples. Sodium benzoate the initial rate of serumloss. The coefficientsA and B, for
(0.2% basedon the addedwater) was added as a preservative. the preliminaryexperiments, arepresented in Table1. As can
At intervals, the combined tubeswere removed from the desiccator, be seenfrom F ig. 2 andTable1, the sampleweightaffected
the condensedmoisture on the exterior of the holder tube was wiped both the rateandthe final amountof serumloss. W ith a cor-
off, the screentube was carefully separatedfrom the holder tube, and
the weight of the holder tube with accumulatedserum was measured. relationcoefficientR* = 0.989thefollowinglinearrelationship
After each weighing, the screen tube was replaced in its holder and was foundto describethe inverseof the initial rateof serum
returned to the desiccator. Weighing intervals of 1, 2, 4, 24, and 48 loss(coefficientA, Table1) asa functionof thesampleweight
hr and 1, 2, 4 wk provided sufficient data to generatea smooth curve (SW in grams)
for the ketchup samplesstudied. Other ketchup formulations may re-
quire variations of this schedule. The test was considered complete A = 0.0370SW - 0.0495 (2)
when two consecutivemeasurements were the same. The percentserum
loss (SL) was calculated from From the aboveexpression,as the sampleweight increased,
the initial rateof separation (l/A) decreased.
This was prob-
SL = Serum weight ably dueto the fact that the averagedistancethe serumhasto
x 100
Ketchup weight flow beforeseparation was furtherfor largersamplesize.
The percentserumloss after 932.5hours(FSL) correlated
Each test was performed in triplicate. with sampleweightthroughthe following expression
1
Ketchup pouches - = 0.0487& + 0.0189
FSL
In order to investigate the separationof serum as it occurs in the
pouches, transparentpouches, of dimensions similar to commercial with a correlationcoefficientR* = 0.988.
ones (flat outside dimensions 4 x 7.5 cm), were made. The flat stock Equation(3) indicatesthat as sampleweightincreased,the
material used for the pouches was composed of nonheat-sealable, amountof serumloss(at 932.5hours)increased, approaching
nitrocellulose-coated,cellophanewhich was adhesively laminated on a lim iting valueof 5 3 %for theparticularketchupsamplestud-
one side to 2.0 mil clean, medium density, polyethylene. The pouches ied. Theincreaseof serumlosswith increasing sampleweight
were fabricated so that the polyethylene was the heat sealable inner maybe dueto the fact that a certainamountof serum,depen-
layer, as used by McCormick and Company, Inc. Poucheswere cold
filled with 9-log ketchup, allowing for a headspacevolume, and the dentonly on the crosssectionalareaof the surfacethrough
top sealed using a bartype heat-sealer. which the serumflows, is held by the porousbed which is
Preliminary data indicated pouchesfilled from the same sub-batch createdby the structuralsolidsof the ketchup.An additional
of ketchup had different degreesof serum separation, depending on reasonm ightbe the changeof samplegeometrythat hasbeen
size and position of the bubble resulting from the air incorporation as observedfor large samples(~8 grams),from cylindricalto

Volume 55, No. 6, 1 QQO-JOURNAL OF FOOD SCIENCE- 1627

 SERUM SEPN POTENTIAL OF TOMATO KETCHUP.. .

Fig. 3-Effect of air bubble size and position on serum separation of ketchup in pouches.

50
of 5 replicates)was found. The final form of the test, as it is
1 describedin the Materialsand MethodsSectiongave a varia-
40 ?+=+- 0 4- -- -__------
__.-.-. ----4--O tion in the rangeof 1 to 3% for most subsequent experiments
z : . --. .-: -..-..-.-. - _.__.----.
-____. (Stoforos,1984).
0 IP l ;-..--

A 30 / :./
-o- 23.3 C

5 ,I +p~ -e- 23.3 C

Single serving pouches
(I
; 20 i q -e- 3.9 C

+ 3.9 C The importanceof air bubble size and position on serum

s i
- - -0.6 C
separation of ketchupin pouchescanbe seenfrom Fig. 3. This
-m- -0.6 0
photographwas taken 1 month after the poucheshad been
filled with homogenized commercialketchupsamplesandstored
0 ~,~,,,,/,/~,~,,,~,~,~,~I as shown. In pouch E, where there was no void space,no
0 50 100150200 250 300350400 450 500550600 serumseparation wasobserved. Thebottomrightsideof pouches
B and D showedsmall air bubblesalmostfilled with serum.
TIME (hours) From pouchesA and B, we could seean analogouseffect of
Fig. 4-Effect of temperature on serum separation. (C.B. = Cold slopeof the ketchupsurfacewhich is in contactwith the air
Break, H.B. = Hot Break) bubble.In pouchB, wherethe ketchupair interfacewas held
in horizontalposition, no serumwas observedon top. How-
ever, therewas someserumon the top right side of pouch A
Table Z-Coefficients associated with Eq. (1) for the experiments study- wherethe ketchupwas slightly mounded.PouchC illustrated
ing the effect of storage temperature
the role of the air bubbleas a serum-holdingshell.
Sample ,6,, lh4) B R2
It canbe inferred,from Fig. 3, that naturalserumseparation
Cold Break 23.3 0.0164 0.0242 1.000
for ketchupin poucheswasdueto drainageof theserumthrough
Cold Break 3.9 0.0623 0.0246 0.998 the solidsmatrix ratherthanto the settlingof insolublesolids.
Cold Break -0.6 0.0926 0.0249 0.991 We could alsoconcludethat the developedtest simulatedthis
Hot Break 23.3 0.1211 0.0245 0.996 phenomenon. The functionof the screenusedin our testwas
Hot Break 3.9 0.2105 0.0314 0.941 only to supportthe ketchupsample.The filtration of the
Hot Break -0.6 0.2371 0.0321 0.962
serumwas donethroughthe insolublesolids of the ketchup.
The chosenscreensizewas the one with maximumopenings
able to hold every ketchupsamplestudied(Stoforos,1984).
conical.A shrinkageof the ketchupresultedin an increasein The minimum size of perforationsthroughwhich the whole
the exposedsurfaceof the sample.Note, that this effect was samplewould start to flow was not the samefor all the sam-
also dependent on the screentube dimensions. ples. There were samplesthat did not flow through4 mm*
From the abovediscussion,it is clearthat the sampleweight perforations.However,significantdifferenceswere observed
was a factorthat shouldbe standardized duringthe serumsep- betweenvarious samples(for example,comparinghomoge-
arationtests. Wishing to (1) maximizethe amountof final nizedwith nonhomogenized ketchups).Thoseresultswill be
serumseparation,in order to better distinguishbetweendif- reportedlater.
ferentketchupsamples,(2) minimizethetime requiredto reach
the final separation,and (3) conservematerial,the S-g sample
weight was selectedas the standardsampleweight for the Effect of storage temperature
proposedserumseparationtest.
During developmentof the test, severalexperimentswere In ketchuppouches,we observedthat loweringstoragetem-
performed.In one, the test was performedoutsidethe desic- peratureslowed serumseparation.To examinethe effect of
cator. In another,the screentubedid not havethe flat portion temperature on serumseparation,the separationtest was per-
for venting(Fig. l), andin a third, the entirescreentubewas formedat threedifferenttemperatures,(23.3,3.9, and -0.6),
placedinsidethe holdertube and coveredwith a plasticstop- on hot breakand cold breakketchupsamples.The resultsare
per. In theseexperiments,a variationof 20 to 50% (expressed presentedin Fig. 4.. The correspondingcoefficientsassociated
as the percentof one standarddeviationon the averagevalue with Eq. (1) are presentedin Table 2. For both hot and cold

7628-JOURNAL OF FOOD SCIENCE-Volume 55, No. 6, 1990


1 .,I,.,~,~,.,~,.,
3.30 3.35 3.40 3.45 3.50 3.55
1 /Tabs ( 1 /KM 1000
Fig. 5-Arrhenius plot showing effect of temperature
rate of serum separation.
break samples,the initial rate of serumloss (l/A, Table 2)
followedthe ArrheniusEquation(Fig. 5).
With a correlationcoefficientR* = 1.000,the resultsfor the
hot breaksampleswere describedby
l/A = 1.86x lo4 exp(- 2.29x 103!T,,,)
for Tabsbeingthe absolutetemperature
(K) and l/A in hour-.
For the cold break sample,the Arrheniusexpressionwith
an R*=0.999 was
l/A = 1.93x lOlo exp(-5.80x 103/T&
Thoughthe initial rate of serumseparationdecreasedas tem-
peraturedecreased, the final amountof serumlosswas almost
independentof storagetemperature.
Gravity sedimentation test
No correlationwas foundbetweenresultsusingthe gravity
sedimentationtest (performedon samplesdilutedwith water
or artificial serum)and eitherthe serumseparationtest or the
serumseparationas it occurredin pouchesof ketchup(Sto-
foros, 1984).The gravity sedimentation test bettersimulated
the serumseparationof ketchupin bottles,which is probably
due to the settlingof the solidsmatrix, and resultsin a layer
of serumabovethe product.This confirmsthat serumsepa-
rationin pouches.isdueto liquid drainage,andthat the serum
separationtest is a more appropriatetest.
SUMMARY
A TEST simulatingserum separationof tomato ketchupin
individualservingpoucheswas developed.The ketchupsam-
ple was supportedby a screen,and the serumdrainedthrough
the insolublesolidsmatrix in a mechanismsimilar to that oc-
curring in naturalseparationin pouches.In contrastto previ-
ouslyusedtests,this testquantifiedboth rateandfinal amount
of serumloss. A saturation-likemodel correlatedserumloss
with time, eliminatingthe needfor prolongedexperiments.
By meansof the test, the effect of storagetemperatureon
serumseparation was studied.Althoughreducingstoragetem-
peraturedecreased initial rate of separation,the final amount
of serumlosswas independent of temperature.
3.60 3.65 3.70
REFERENCES
on initial
Anonymous, 1953. United States Standards for Grades of Tomato Catsu
4th issue, effective August 31 U.S,Dept. of Agriculture, Agricu P -
tural Marketin son, DC.
ada, N. 1985. Tomato products: A new
serum separation measurement. J. Food Sci. 50: 1493.
Davis, R.B., de Weese, D., and Gould, W.A. 1954. Consistency measure-
ments of tomato puree. Food Technol. 8: 330.
Gould, W.A. 1983. Tomato Production, Processing, and Quality Evaluation,
2nd ed. AVl Publishing Co., Inc., Westport, CT.
Marsh, G.L., Leonard, S.J., Buhlert, J.E., and Vilas, M.R. 1979a. Yield
and quality of catsup produced to a standard solids and consistency level.
I. Method of determining the amount of tomato solids required. J. Food
Proc. Pres. 3: 189. -
(4) Marsh, G.L., Leonard, S.J., and Buhlert, J.E. 1979b. Yield and uality of
catsup reduced to a standard solids and consistency level. II. 9 nfluence
of hand pi ng practices, break temperature and cultivar. J. Food Proc. Pres.
3: 195.
Marsh, G.L., Wolcott, T.K., Heil, J.R., and Merson, R.L. 1985.1984 processing
tomato variety trials. Progress Report to California League of Food Pro-
cessors. Univ. of California, Davis, CA.
McColloch, R.J,, Nielsen, B.W., and Bearens, E.A. 1950. Factors influenc-
ing the uahty of tomato paste. II. Pectic changes during processing.
(5) Food TeeR nol. 4: 339.
Nelson, A.I., Steinberg, M.P.,, McGill, J.N., and Vetter, J.L. 1957. Effect
of continuous steam injection of tomato juice on film deposition during
subse uent concentration. Food Technol. 11: 406.
Palma, % .R. 1983. Personal communication.
juana, Mexico.
Instituto Technologlco de Ti-
Robinson, W.B., Kimball,, L.B., Ransford, J.R., Moyer, J.C., and Hand, D.B.
1956. Factors influenmng the degree of settling m tomato juice. Food
Technol. 10: 109.
Shomer, I., Lindner, P., and Vasiliver, R. 1983. The mechanism which
enables the cell wall to retain homogeneous ap earance of tomato juice.
Institute of Technology and Storage of A
E;ailResearch Organization, No. 764-E. T
Smit, C.J.B. and Nortje, B.K. 1958. Observations on the consistency of
tomato aste. Food Technol. 12: 356.
Stoforos, RT.G. 1984. Serum Separation of Tomato Ketchu
Dept. of Food Science & Technology, Univ. of California,
. MS. thesis,
% avis, CA.
Twigg, B.A. 1969. Consistency and-Serum Separation of Catsup. Ph.D.
dissertation. Univ. of Ma&and. Colleee Park. Marvland. MD.
Ms received 7)18/89; revised 3/8/90; acc&ed S/3/90.
Grateful acknowledgement
sumort of this work.
is made to McCormick and Company Inc. for financial
Volume 55, No. 6, 1990-JOURNAL OF FOOD SCIENCE-1629