Linieritas Nipasol

penimbangan 10.05
volume labu 50
Konsentrasi (ppm) 201

pengenceran
pipet 0.5
volume labu 25
Konsentrasi (ppm) 4.02

Konsentrasi (ppm) Luas Area

3.2160 174313
Linieritas Nipasol

Luas Area
3.6180 198985
4.0200 213555 300000
4.4220 242917 250000
4.8240 266710
200000
a -9430.0000000001
b 56897.0149253731 150000
r 0.9959 100000
50000
0
3.0000 3.20003.40003.6000 3.80004.0000 4.20004.40004.6000 4.80005.0000
Konsentrasi (ppm)

Noise = 1 x 213555 = 2135.55

100 Rasio Signal/N oise

Konsentrasi (ppm) Rasio Signal/Noise

3.2160 81.62
3.6180 93.18
4.0200 100.00
4.4220 113.75
Linieritas Nipasol
4.8240 124.89 140.00
a -4.4157242865 120.00
f(x) = 26.64279222x - 4.4157242865
b 26.64279222 100.00 R² = 0.9917636439
r 0.9959 80.00
60.00
40.00
20.00
0.00
3.00003.20003.40003.60003.80004.00004.20004.40004.60004.80005.0000
Konsentrasi (ppm)

Perhitungan Untuk LOD dan LOQ

y = 56897.0193-9430

Konsentrasi (ppm) Luas Area Yi (Yi-luas area) (Yi-luas area)2

3.2160 174313 182981.795873 8669 75148021.8930677
3.6180 198985 205854.395873 6869 47188599.6642095
4.0200 213555 228726.995873 15172 230189458.77965
4.4220 242917 251599.595873 8683 75387471.0991708
4.8240 266710 274472.195873 7762 60251684.775587
a -9430.0000000001 ∑ (Yi-luas area)2 488165236.211685
b 56897.0149253731 ∑ (Yi-luas area)2/N-2 162721745.403895
r 0.9959 SD = √∑ (Yi-luas area)2/N-2 12756.24
LOD = 3 SD/b 0.67
LOQ = 10SD/b 2.24
4.60004.80005.0000

04.60004.80005.0000
 Validasi Kadar vomerin suspensi

Spesifisitas nipasoll
No Area Kadar
1 0 0%
2 0 0% Area Standard
3 0 0%

Area Standard 218806

Bobot Standard 10.05 mg
Kadar Standard 100.90 %
Fp 0.2 x
LC 1 mg
BJ vomerin 1.112 1
volume sediaan 5
Akurasi
No Konsentrasi penimbangan Luas Area Kadar (% ) %Recovery
1 80% 8.6172 170558 102.00 97.64
2 80% 8.5930 173465 104.03 99.58
3 80% 8.5786 173122 104.00 99.55
4 100% 10.6875 213208 102.81 98.41
5 100% 10.6485 214025 103.58 99.15
6 100% 10.5032 213691 104.85 100.36
7 120% 12.8907 259999 103.94 99.50
8 120% 12.7952 260615 104.97 100.48
9 120% 12.8647 260997 104.55 100.08
Rata-rata 103.86 99.42
sd 0.96 0.92
RSD 0.92 0.92
Presisi Sistem
No Konsentrasi penimbangan Luas Area Kadar (% )
1 100% 10.5 212972 104.34
2 100% 10.5 213356 104.53
3 100% 10.5 213434 104.56
4 100% 10.5 213261 104.48
5 100% 10.5 213247 104.47
6 100% 10.5 213171 104.44
Rata-rata 213240 104.47
sd 160 0.08
RSD 0.08 0.08

Validasi Kadar nipasol dalam vomerin (Hari 2) Area Standard

212285
212148
Area Standard 212534 212205
Bobot Standard 10.00 mg 213194
Kadar Standard 100.90 % 212742
Fp 0.2 x 212629
LC 1 mg 212533.833333333
BJ nipasol 1.112 1 402
volume sediaan 5 0.19
Akurasi
No Konsentrasi penimbangan (mg) Luas Area Kadar (% ) %Recovery
1 80% 8.6 178294 109.23 101.99
2 80% 8.6 179727 110.42 103.10
3 80% 8.6 180281 110.94 103.59
4 100% 10.7 216426 106.91 99.82
5 100% 10.7 216637 107.04 99.95
6 100% 10.5 216275 108.71 101.50
7 120% 12.9 255150 104.49 97.57
8 120% 12.8 255180 105.29 98.31
9 120% 12.9 255005 104.64 97.71
Rata-rata 107.52 100.39
sd 2.44 2.27
RSD 2.27 2.27
Presisi Antara
No Konsentrasi penimbangan (mg) Luas Area Kadar (% )
1 100% 10.7 216251 106.82
2 100% 10.7 216520 106.95
3 100% 10.7 216542 106.96
4 100% 10.7 216388 106.89
5 100% 10.7 216436 106.91
6 100% 10.7 218759 108.06
Rata-rata 216816 107.10
sd 958 0.47
RSD 0.44 0.44
Area Standard
218617 1.444 25125.398
219495 1.44 25207.316
219166 1.447 25218.225
219161 1.445 24498.741
218147 1.434 25058.708
218251 1.432 25096.098
218806.167 1.44033 25034.081
549 0 270
0.25 0.43 1.08

konsentrasi
3.44688
3.4372
3.43144
4.275
4.2594
4.20128
5.15628
5.11808
5.14588

1.319 51510.71
1.326 49855.5
1.325 49898.94
1.334 49187.48
1.329 49968.85
1.335 49674.23
1.328 50015.95
0.01 784.74
0.45 1.57

konsentrasi
3.44688
3.4372
3.43144
4.275
4.2738
4.20128
5.15628
5.11808
5.14588
 Validasi Kadar Metoclopramide Dalam Metoclopramide 10 mg/2 ml Injection

Bobot Standard 10.05 mg

Kadar Standard 100.90 %
Fp 0.2 x
Label klaim 1 mg
BJ Nipasol 1.112 1
volume sediaan 5
Robustnes fase gerak
pH 4.3

Presisi Standar
No Konsentrasi Berat Standar (mg) Luas Area
1 100% 10.00 220469
2 100% 10.00 222284
3 100% 10.00 222116
4 100% 10.00 222347
5 100% 10.00 221713
6 100% 10.00 222459
Rata-rata 221898
sd 747
Rsd 0.34

Presisi Sampel
No Konsentrasi penimbangan Luas Area Kadar (%)
1 100% 10.7 223740 106.38
2 100% 10.7 223259 106.16
3 100% 10.7 223206 106.13
4 100% 10.7 223246 106.15
5 100% 10.7 223030 106.05
6 100% 10.7 222997 106.03
Rata-rata 223246 106.15
sd 266 0.13
Rsd 0.12 0.12

Robustnes fase gerak

ppH 4,1

Presisi Standar
No Konsentrasi Berat Zat Uji (mg) Luas Area
1 100% 10.00 217064
2 100% 10.00 221696
3 100% 10.00 224836
4 100% 10.00 226875
5 100% 10.00 221600
6 100% 10.00 221587
Rata-rata 222276
sd 3351
Rsd 1.51

Presisi Sampel
No Konsentrasi penimbangan Luas Area Kadar (%)
1 100% 10.7 225277 106.93
2 100% 10.7 225183 106.89
3 100% 10.7 224853 106.73
4 100% 10.7 224323 106.48
5 100% 10.7 225192 106.89
6 100% 10.7 224643 106.63
Rata-rata 224912 106.76
sd 376 0.18
Rsd 0.17 0.17
 Validasi Kadar nipasol dalam vomerin

Bobot Standard 10.05 mg

Kadar Standard 100.90 %
Fp 0.2 x
Label klaim 1 mg
BM Metoclopramide 1.112 1
voume sediaan 5
Robustnes flow 0.8 mL/min

Presisi Standar
No Konsentrasi Berat Standar (mg) Luas Area
1 100% 10.05 278006
2 100% 10.05 268780
3 100% 10.05 269848
4 100% 10.05 273704
5 100% 10.05 270236
6 100% 10.05 271356
Rata-rata 271988
sd 3391
Rsd 1.25

Presisi Sampel
No Konsentrasi berat sampel (mg) Luas Area Kadar (%)
1 100% 10.7 272181 105.58
2 100% 10.7 272392 105.66
3 100% 10.7 272472 105.70
4 100% 10.7 272816 105.83
5 100% 10.7 272374 105.66
6 100% 10.7 272717 105.79
Rata-rata 272492 105.70
sd 235 0.09
Rsd 0.09 0.09

Robustnes flow 1.2 mL/min

Presisi Standar
No Konsentrasi Berat Zat Uji (mg) Luas Area
1 100% 10.05 180395
2 100% 10.05 183282
3 100% 10.05 182421
4 100% 10.05 181928
5 100% 10.05 182105
6 100% 10.05 181710
Rata-rata 181974
sd 948
Rsd 0.52

Presisi Sampel
No Konsentrasi Volume Zat Uji (mL) Luas Area Kadar (%)
1 100% 10.0 165496 102.47
2 100% 10.0 165442 102.44
3 100% 10.0 165763 102.63
4 100% 10.0 165433 102.43
5 100% 10.0 165388 102.40
6 100% 10.0 165684 102.59
Rata-rata 165534 102.49
sd 153 0.09
Rsd 0.09 0.09
Validasi Kadar Metoclopramide Dalam Metoclopramide 10 mg/2 ml Injection (Ruggednes)

No Konsentrasi %Recovery Hari 1 %Recovery Hari 2

1 80% 97.64 101.99

2 80% 99.58 103.10

3 80% 99.55 103.59

4 100% 98.41 99.82

5 100% 99.15 99.95

6 100% 100.36 101.50

7 120% 99.50 97.57

8 120% 100.48 98.31

9 120% 100.08 97.71

Rata-rata 99.42 100.39

sd 0.92 2.27

Rsd 0.92 2.27

Rata-rata 99.90

sd 1.76

Rsd 1.76
 Kestabilan Larutan
RT Standard Area Standar RT Sampel Area Sampel
Jam ke Jam ke
Nipasol Nipasol Nipasol Nipasol
1 1
(Tgl: 13 May 15, (Tgl: 13 May
8.355 227120 8.363 227596
4:17:57 PM ) 15, 4:24:26 PM)

2 8.347 227434 2 8.327 227015

3 8.334 227058 3 8.327 226588
4 8.309 225054 4 8.317 227278
5 8.325 226916 5 8.328 227770
6 8.327 227361 6 8.324 227676
7 8.323 227331 7 8.332 227746
8 8.300 225415 8 8.326 227733
9 8.308 227192 9 8.321 227572
10 8.307 227382 10 8.316 228101
11 8.301 227233 11 8.322 227858
12 8.298 227089 12 8.322 227988
13 8.326 226108 13 8.325 228394
14 8.332 226278 14 8.333 228926
15 8.320 228134 15 8.316 228901
16 8.323 226561 16 8.321 228930
17 8.329 185578 17 8.310 62395
18 8.306 187174 18 8.308 66130
19 8.299 161269 19 8.307 63865
20 8.303 176726 20 8.314 70609
21 8.297 178781 21 8.304 62416
22 8.306 168497 22 8.296 62458
23 8.295 166663 23 8.294 57738
24 24
(Tgl: 14 May 15, (Tgl: 14 May
8.303 159178 8.295 78631
4:10:39 PM) 15, 4:17:09 PM)

Rata-rata 8.316 208897 Rata-rata 8.319 173763

sd 0.017 26607 sd 0.015 78261
%RSD 0.20 12.74 %RSD 0.18 45.04
 Linieritas I Xanthorrhizol

Konsentrasi (ppm) Luas Area

113.3863 128554
Linieritas Leucocyanidins

Luas Area
127.7011 145296
141.8461 160466 1400000
155.5950 181439 1200000 f(x) = 7759.4840022273x + 97373.6429791924
169.7400 196766 1000000 R² = 0.9902641714
a 97374 800000
b 7759.5
600000
r 0.9951
400000
200000
0
90 100 110 120 130 140 150 16
Konsentrasi (ppm)

Noise = 1 x 160466 = 1604.66

100 Rasio Signal/N oise

Konsentrasi (ppm) Rasio Signal/Noise

113.3863 80.11
127.7011 90.55
141.8461 100.00
Linieritas Xanthorrhizol
155.5950 113.07 140
169.7400 122.62 120
f(x) = 0.7283089814x + 9.1395379792
a 9.1395 100 R² = 0.9902641714
b 0.7283 80
60
40
20
0
90 100 110 120 130 140 150 160
Konsentrasi (ppm)

Perhitungan Untuk LOD dan LOQ

y=7759.5X+97374

Konsentrasi (ppm) Luas Area Yi (Yi-luas area) (Yi-luas area)2

102.0000 888679 888843 164 26896
114.7500 1004849 987776.625 -17072 291465988.140625
127.5000 1065411 1086710.25 21299 453658050.5625
140.3010 1178023 1186039.6095 8017 64266027.8754906
153.0000 1296973 1284577.5 -12396 153648420.25
a 97374 ∑ (Yi-luas area)2 963065382.828616
b 7759.5 ∑ (Yi-luas area) /N-2 2
321021794.276205
r 0.9951 SD = √∑ (Yi-luas area)2/N-2 17917.08
LOD = 3 SD/b 6.93
LOQ = 10SD/b 23.09
thorrhizol

+ 97373.6429791924

0 140 150 160

)

5379792

140 150 160

)
 Linieritas 2 Xanthorrhizol

Konsentrasi (ppm) Luas Area

102.0255 888479
Linieritas Xanthorrhizol

Luas Area
114.7500 1003306
127.5255 1063214 1400000
140.3010 1178113 1200000 f(x) = 7750.4257257455x + 97322.684111444
153.0255 1295386 1000000 R² = 0.9901633296
a 97323 800000
b 7750.4
600000
r 0.9951
400000
200000
0
90 100 110 120 130 140 150
Konsentrasi (ppm)

Noise = 1 x 1063214 = 10632.14

100
Rasio Signal/N oise
Konsentrasi (ppm) Rasio Signal/Noise
102.0255 83.57
114.7500 94.37
127.5255 100.00
140.3010 110.81
Linieritas Xanthorrhizol
153.0255 121.84 140
a 9.1536 120
f(x) = 0.7289619706x + 9.1536307941
b 0.729 100 R² = 0.9901633296
80
60
40
20
0
90 100 110 120 130 140 150
Konsentrasi (ppm)

Perhitungan Untuk LOD dan LOQ

y=7750.4X+97323

Konsentrasi (ppm) Luas Area Yi (Yi-luas area) (Yi-luas area)2

102.0255 888479 888061.4352 -418 174360.3621991
114.7500 1003306 986681.4 -16625 276377325.16
127.5255 1063214 1085696.6352 22483 505468885.5363
140.3010 1178113 1184711.8704 6599 43545090.55599
153.0255 1295386 1283331.8352 -12054 145302889.0256
a 97323 ∑ (Yi-luas area)2 970868550.64
b 7750.4 ∑ (Yi-luas area) /N-2 2
323622850.2133
r 0.9951 SD 17989.52
LOD = 3 SD/b 6.96
LOQ = 10SD/b 23.21
ol

izol
57455x + 97322.684111444
6

130 140 150 160

rasi (ppm)

+ 9.1536307941

130 140 150 160

rasi (ppm)
 Linieritas 3 Xanthorrhizol

Konsentrasi (ppm) Luas Area

102.0255 885168
Linieritas Xanthorrhizol

Luas Area
114.7500 1009390
127.5255 1089375 1400000
140.3010 1170908 1200000 f(x) = 7635.944017315x + 115474.877905409
153.0510 1291616 1000000 R² = 0.9925874085
a 115475 800000
b 7635.9
600000
r 0.9963
400000
200000
0
90 100 110 120 130 140 150
Konsentrasi (ppm)

Noise = 1 x 1089375 = 10893.75

100
Rasio Signal/N oise
Konsentrasi (ppm) Rasio Signal/Noise
102.0255 81.25
114.7500 92.66
127.5255 100.00
140.3010 107.48
Linieritas Xanthorrhizol
153.0510 118.56 140
a 10.6 120
f(x) = 0.700947242x + 10.6001035369
b 0.7009 100
R² = 0.9925874085
80
60
40
20
0
90 100 110 120 130 140 150
Konsentrasi (ppm)

Perhitungan Untuk LOD dan LOQ

y=7635.9X+115475

Konsentrasi (ppm) Luas Area Yi (Yi-luas area) (Yi-luas area)2

102.0255 885168 894531.51545 9364 87675421.5823877
114.7500 1009390 991694.525 -17695 313129835.475628
127.5255 1089375 1089246.96545 -128 16392.8459936979
140.3010 1170908 1186799.4059 15891 252536781.478552
153.0510 1291616 1284157.1309 -7459 55634728.2509385
a 115475 ∑ (Yi-luas area)2 708993159.6335
b 7635.9 ∑ (Yi-luas area) /N-2 2
236331053.211167
r 0.9963 SD 15373.06
LOD = 3 SD/b 6.04
LOQ = 10SD/b 20.13
l

+ 115474.877905409

130 140 150 160

ppm)

6001035369

130 140 150 160

ppm)