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HPLC

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konsentrasi

(g/mL)
No
Tmp
Smx
1
10
20
30
40
50
2
10
20
30
40
50
3
10
20
30
40
50

Luas puncak
Tmp
10
20
30
40
50
10
20
30
40
50
10
20
30
40
50

Smx
950618
1337851
1888024
2258314
2793831
980266
1395980
1841638
2254895
2817963
955563
1339299
1837407
2228038
2802854

Persamaan regresi

Tmp
1274543 a = 46366
1752549 b = 46069
2280876 r = 0,996
2808316
3228932
1238125 a = 49785
1700055 b = 45343
2220647 r = 0,996
2737969
3263260
1218851 a = 45763
1717012 b = 45833
2237141 r = 0,995
2770067
3245339

Smx
a = 77968
b = 49645
r = 0.998

3000000

2500000

2000000

1500000
Luas Puncak Tm

a = 70555
b = 50882
r = 0.999

1000000

500000

a = 70587
b = 51060
r = 0,999

3500000

3000000

10
20
30
40
50

2500000

980266
1395980
1841638
2354895
2817963

2000000

Luas Puncak
Sm
1500000

1000000

500000

kadar (ppm) luas area(auc)


10
980266
20 1395980
30 1841638

kadar (ppm) luas


10
20
30

area(auc)
1238125
1700055
2220647

40
50

2254895
2817963

40
50

2737969
3263260

3000000
f(x) = 45343.09x + 497855.7
R = 0.9965074419

2500000
2000000
1500000
Luas Puncak Tmp

luas area(auc)

1000000

Linear (luas
area(auc))

500000
0
0

10

20

30

40

50

60

Konsentrasi (g/mL)

3500000
f(x) = 50881.84x + 705556
R = 0.9994510221

3000000
2500000
2000000
Luas Puncak
Smx
1500000

luas area(auc)

1000000

Linear (luas
area(auc))

500000
0
5

10

15

20

25

30

35

Konsentrasi (g/mL)

40

45

50

55

No

konsentrasi
(g/mL)
Tmp
Smx
2
10
20
30
40
50

Luas puncak

Persamaan regresi

Tmp
Smx
Tmp
10
980266 1238125 a = 49785
20 1395980 1700055 b = 45343
30 1841638 2220647 r = 0,996
40 2254895 2737969
50 2817963 3263260

Persamaan regresi
Smx
a = 70555
b = 50882
r = 0.999

Uji Kesesuaian Sistem 10 ppm


tR (menit)
luas area (AUC)
tinggi puncak
No.
tmp
smx
tmp
smx
tmp
smx
1
0.95
2.143
980266 1238125
150759
119236
2
0.955
2.141
982421 1274400
154654
120346
3
0.959
2.15
984421 1273588
155654
120329
SD
0.004509 0.004726 2077.982 20712.96 2586.247 636.0081
Rata-rata 0.954667 2.144667 982369.3 1262038
153689 119970.3
RSD
0.47%
0.22%
0.21%
1.64%
1.68%
0.53%

Uji Kesesuaian Sistem 50 ppm


tR (menit)
luas area (AUC)
tinggi puncak
No.
tmp
smx
tmp
smx
tmp
smx
1
1.01
2.173 2817963 3263260
364058
481456
2
1.013
2.18 2793831 3228932
362858
476970
3
1.008
2.183 2802854 3245339
363322
479303
SD
0.002517 0.005132 12193.23 17169.56 605.116 2243.602
Rata-rata 1.010333 2.178667 2804883 3245844 363412.7
479243
RSD
0.25%
0.24%
0.43%
0.53%
0.17%
0.47%

RSD
parameter
waktu retensi (menit)
luas puncak
tinggi puncak

10 g/mL
50 g/mL
tmp
smx
tmp
smx
0.47%
0.22%
0.25%
0.24%
0.21%
1.64%
0.43%
0.53%
1.68%
0.53%
0.17%
0.47%
0.79%

0.4
0.6
0.65
0.55

konsentrasi 20 ppm
tR (menit)
luas area (AUC)
tinggi puncak
No.
tmp
smx
tmp
smx
tmp
smx
1
1.013
2.177 1337851 1752549
280504
262292
2
1.018
2.178 1328413 1728731
285837
257087
3
1.014
2.172 1339299 1727012
283156
260326
SD
0.0026458 0.003215 5911.536 14273.46 2666.513 2628.317
Rata-rata
1.015 2.175667 1335188 1736097 283165.7 259901.7
RSD
0.26%
0.15%
0.44%
0.82%
0.94%
1.01%

konsentrasi 30 ppm
tR (menit)
luas area (AUC)
tinggi puncak
No.
tmp
smx
tmp
smx
tmp
smx
1
1.01
2.166 1841638 2220647
303982
414349
2
1.005
2.167 1837407 2237141
302642
418478
3
1.008
2.164 1838841 2203708
301047
413338
SD
0.0025166 0.001528 2151.779 16716.99 1469.345 2723.061
Rata-rata
1.0076667 2.165667 1839295 2220499
302557 415388.3
RSD
0.25%
0.07%
0.12%
0.75%
0.49%
0.66%

konsentrasi 40 ppm
tR (menit)
luas area (AUC)
tinggi puncak
No.
tmp
smx
tmp
smx
tmp
smx
1
1.007
2.207 2228038 2770067
309724
356018
2
1.013
2.211 2247721 2723211
310550
351023
3
1.01
2.213 2254895 2737969
310821
348041
SD
0.003 0.003055 13905.55 23956.78 571.4202 4030.61
Rata-rata
1.01 2.210333 2243551 2743749
310365
351694
RSD
0.30%
0.14%
0.62%
0.87%
0.18%
1.15%

replikasi
akurasi tmp smx
80%
1
2
3
100%
1
2
3
120%
1
2
3

Luas Area (AUC) A


Kadar A (ppm)
Luas Area (AUC) B
tmp
smx
tmp
smx
tmp
smx
1 1460675 2041879 31.116 38.743
1054413 1464400
2 1468655 2048777 31.292 38.879
1054413 1464400
3 1468786 2028149 31.295 38.473
1054413 1464400
1 1955002 2414055 42.018 46.058
1054413 1464400
2 1959185 2419506 42.110 46.165
1054413 1464400
3 1947970 2423346 41.863 46.240
1054413 1464400
1 2419686 3079952 52.266 59.145
1054413 1464400
2 2416100 3092798 52.187 59.397
1054413 1464400
3 2425224 3089891 52.388 59.340
1054413 1464400

tmp
a=
b=
r2=

49785
45343
0,996

smx
a=
b=
r2=

70555
50882
0,999

kadar B (ppm)
Luas Area (AUC) C
kadar C (ppm)
perolehan kembali (%)
tmp
smx
tmp
smx
tmp
smx
tmp
smx
22.1562 27.394
459918
642565
9.045 11.242
99.056
100.956
22.1562 27.394
459918
642565
9.045 11.242 101.002
102.162
22.1562 27.394
459918
642565
9.045 11.242 101.034
98.556
22.1562 27.394
938841 1020876 19.607 18.677 101.297
99.930
22.1562 27.394
938841 1020876 19.607 18.677 101.768
100.504
22.1562 27.394
938841 1020876 19.607 18.677 100.506
100.908
22.1562 27.394 1428314 1694691 30.402 31.920
99.038
99.471
22.1562 27.394 1428314 1694691 30.402 31.920
98.778
100.262
22.1562 27.394 1428314 1694691 30.402 31.920
99.440
100.083

SD
tmp

smx

tmp

Rata-Rata
smx

tmp

% RSD
smx

1.133

1.836

100.364

100.558

1.13%

1.83%

0.637

0.491

101.190

100.447

0.63%

0.49%

0.333

0.415

99.086

99.939

0.33%

0.42%

Kadar Sampel Sesudah


kadar sebelum pengenceran
Luas
Puncak
(AUC)
Pengenceran
10x
(ppm)
10x dalam 50 ml (ppm)
Serbuk
no Tablet (mg) tmp
smx
tmp
smx
tmp
1
614.5 2218685 2513095
47.833
48.004
478.332
2
614.8 2229351 2500031
48.068
47.747
480.684
3
614.7 2214916 2501325
47.750
47.773
477.501
4
615.1 2209160 2514126
47.623
48.024
476.231
5
615 2216861 2515794
47.793
48.057
477.930
SD
1.628
Rata-rata
478.135
RSD
0.34%
tmp
a=
b=
r2=

49785
45343
0,996

smx
a=
b=
r2=

70555
50882
0,999

r sebelum pengenceran
Kandungan tmp dan smx
x dalam 50 ml (ppm)
dalam 480 mg
kandungan dalam tablet (%)
smx
tmp
smx
tmp
smx
480.040
80.279
399.967
100.349
99.992
477.473
79.886
402.117
99.858
100.529
477.727
80.419
401.903
100.523
100.476
480.243
80.633
399.798
100.791
99.949
480.571
80.347
399.525
100.433
99.881
1.485
0.273
1.243
0.341
0.311
479.211
80.313
400.662
100.391
100.166
0.31%
0.34%
0.31%
0.34%
0.31%

No
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
SD
Rata2
RSD

Berat Tablet (mg)


616.3
616.4
625.3
616.8
612.9
607.2
609.9
629.8
616.5
603.4
606.8
626.7
622.5
605.8
615.9
618.4
607.8
610.8
612.4
613.7
7.23
614.77
1.18%

No

XX

X (ppm) Xi
1
10
2
20
3
30
4
40
5
50
30

tmp
a=
b=
r2=

No

XX

Xi-XX
100
400
900
1600
2500
5500

49785
45343
0,996

X (ppm) Xi
1
10
2
20
3
30
4
40
5
50
30

100
400
900
1600
2500
5500

(Xi-XX)
-20
-10
0
10
20

400
100
0
100
400
1000

smx
a=
b=
r2=

70555
50882
0,999

Xi-XX

(Xi-XX)
-20
-10
0
10
20

400
100
0
100
400
1000

Yi

Yc

980266
1395980
1841638
2254895
2817963

Yi
Yc
1238125
1700055
2220647
2737969
3263260

(Yi-Yc)
503215
477051
956645
439335
1410075
431563
1863505
391390
2316935
501028

579375
1088195
1597015
2105835
2614655

(Yi-Yc)
658750
611860
623632
632134
648605

(Yi-Yc)
2.27578E+11
193015242225
186246622969
153186132100
251029056784
1.01105E+12

(Yi-Yc) / (n-2)

(Yi-Yc)
4.33952E+11
374372659600
388916871424
399593393956
420688446025
2.01752E+12

(Yi-Yc) / (n-2)

Sy/x

3.37018E+11 5.80533E+05

Sy/x

6.72508E+11 8.20066E+05

n (Xi-xx)

5000

n (Xi-xx)

5000

( Xi/ n (Xi-xx))

1.0488088482

( Xi/ n (Xi-xx))

1.0488088482

Sa

6.08868E+05

Sa

8.60092E+05

Y LOD

Y LOQ

LOD

LOQ

1876389 6138463.515 40.28414 134.2805

Y LOD

Y LOQ

LOD

LOQ

2580276 8.67148E+06 49.32434 169.0366

1
2
3
4
5
XX

tmp
a=
b=
r2=

No
1
2
3
4
5
XX

Y=
A=
B=
R2=

X
10
20
30
40
50
30

Xi
100
400
900
1600
2500
5500

Xi-XX
-20
-10
0
10
20

(Xi-XX)
400
100
0
100
400
1000

72137
50448
0.999

X
10
20
30
40
50
30

Yi
980266
1428413
1841638
2347721
2817963

Yc
5116937
20251337
45475337
80788937
126192137

50479 a = 72137
45947 b = 50448
0,998
r = 0.999
Xi
100
400
900
1600
2500
5500

Xi-XX
-20
-10
0
10
20

53108,829x+178546,667
50479
45947
0.998

(Xi-XX)
400
100
0
100
400
1000

Yi
1238125
1728731
2220647
2723211
3263260

509949
969419
1428889
1888359
2347829

Yc
432343
868461
1441303
1945783
2450263

(Yi-Yc)
-4136671
-18822924
-43633699
-78441216
-123374174

(Yi-Yc) / (n-2)
Sy/x
n (Xi-xx) ( Xi/ n (Xi
(Yi-Yc)
17112046962241
12381E+015 76892010.9326
6000 0.957427
3.5430247E+014
1.9038997E+015
6.1530244E+015
1.5221187E+016
2.3649525E+016

(Yi-Yc)
805782
860270
779344
777428
812997

(Yi-Yc) / (n-2)
Sy/x
n (Xi-xx) ( Xi/ n (Xi
(Yi-Yc)
649284631524 1087361530651 1042766.28765
5000 1.048809
740064472900
607377070336
604394295184
660964122009
3262084591953

903062.095311

Sa

Y LOD

Y LOQ

LOD

LOQ

73618496 220927624 736257093 4377.884 14592.946

Sa

Y LOD

1093663 3331466.53

Y LOQ

10987104

LOD

LOQ

71.408

238.027

10 ppm
Uji Kesesuaian Sistem 10 ppm
No.

tR (menit)
luas area (AUC)
tinggi puncak
tmp
smx
tmp
smx
tmp
smx
1
0.95
2.143 1010266 1238125
150759
119236
2
0.955
2.141 1012421 1274400
154654
120346
3
0.959
2.15 1014421 1273588
155654
120329
SD
0.004509 0.004726 2077.982 20712.96 2586.247 636.0081
Rata-rata 0.954667 2.144667 1012369 1262038
153689 119970.3
RSD
0.47%
0.22%
0.21%
1.64%
1.68%
0.53%

Uji Kesesuaian Sistem 50 ppm


No.

tR (menit)
luas area (AUC)
tinggi puncak
tmp
smx
tmp
smx
tmp
smx
1
1.01
2.173 2817963 3263260
364058
481456
2
1.013
2.18 2793831 3228932
362858
476970
3
1.008
2.183 2802854 3245339
363322
479303
SD
0.002517 0.005132 12193.23 17169.56 605.116 2243.602
Rata-rata 1.010333 2.178667 2804883 3245844 363412.7
479243
RSD
0.25%
0.24%
0.43%
0.53%
0.17%
0.47%

No

konsentrasi
(g/mL)
Tmp
Smx
1
10
20
30
40
50
2
10
20
30
40
50
3
10
20
30
40
50

10
20
30
40
50

1010266
1428413
1841638
2347721
2817963

Luas puncak

Persamaan regresi

Tmp
Smx
Tmp
Smx
10
982421 1274400 a = 47898 a = 77081
20 1337851 1752549 b = 45433 b = 49648
30 1837407 2237141 r = 0,996 r = 0.998
40 2258314 2808316
50 2793831 3228932
10
980266 1238125 a = 50479 a = 72137
20 1428413 1728731 b = 45947 b = 50448
30 1841638 2220647 r = 0,998 r = 0.999
40 2347721 2723211
50 2817963 3263260
10
984421 1273588 a = 48100 a = 74297
20 1339299 1717012 b = 45256 b = 49966
30 1838841 2203708 r = 0,994 r = 0,998
40 2228038 2770067
50 2802854 3245339

konsentrasi 30 ppm

konsentrasi 40 ppm

konsentrasi 20 ppm
tR (menit)
luas area (AUC)
tinggi puncak
No.
tmp
smx
tmp
smx
tmp
smx
1
1.013
2.177 1437851 1752549
280504
262292
2
1.018
2.178 1428413 1728731
285837
257087
3
1.014
2.172 1439299 1727012
283156
260326
SD
0.002646 0.003215 5911.536 14273.46 2666.513 2628.317
Rata-rata
1.015 2.175667 1435188 1736097 283165.7 259901.7
RSD
0.26%
0.15%
0.41%
0.82%
0.94%
1.01%
konsentrasi 30 ppm
No.

tR (menit)
luas area (AUC)
tinggi puncak
tmp
smx
tmp
smx
tmp
smx
1
1.01
2.166 1841638 2220647
303982
414349
2
1.005
2.167 1837407 2237141
302642
418478
3
1.008
2.164 1838841 2203708
301047
413338
SD
0.002517 0.001528 2151.779 16716.99 1469.345 2723.061
Rata-rata 1.007667 2.165667 1839295 2220499
302557 415388.3
RSD
0.25%
0.07%
0.12%
0.75%
0.49%
0.66%
konsentrasi 40 ppm
No.

tR (menit)
luas area (AUC)
tinggi puncak
tmp
smx
tmp
smx
tmp
smx
1
1.007
2.207 2328038 2770067
309724
356018
2
1.013
2.211 2347721 2723211
310550
351023
3
1.01
2.213 2354895 2737969
310821
348041
SD
0.003 0.003055 13905.55 23956.78 571.4202 4030.61
Rata-rata
1.01 2.210333 2343551 2743749
310365
351694
RSD
0.30%
0.14%
0.59%
0.87%
0.18%
1.15%

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