1. Pemilihan sampel
Keseragaman Bobot (g)
0.7580 0.7526 0.7540 0.7573
0.7600 0.7630 0.7584 0.7440
0.7571 0.7677 0.7341 0.7637
0.7476 0.7370 0.7562 0.7530
0.7443 0.7467 0.7577 0.7788
- Penyimpangan 5%
Bobot rata-rata x 5% : 754.56 mg x 5% = 37.728 mg
Batas bawah : 754.56 mg - 37.728 mg = 716.832 mg
Batas atas : 754.56 mg + 37.728 mg = 792.288 mg
- Penyimpangan 10%
Bobot rata-rata x 10% : 754.56 mg x 10% = 75.453mg
Batas bawah : 754.56 mg - 75.453 mg = 679.107 mg
Batas atas : 754.56 mg + 75.453 mg = 830.013 mg
Berdasarkan gambar tersebut dapat dilihat bahwa serapan antara parasetamol (A)
dan ibuprofen (B) saling tumpang tindih pada panjang gelombang antara 220 nm
sampai 240 nm dan berpotongan pada panjang gelombang 230 nm. Sehinggga panjang
gelombang yang digunakan pada sistem KCKT adalah 230 nm.
Replikasi 1 Paracetamol
8000000
7000000
y = 43672x - 823458 a = -823458
6000000 R² = 0,961
b = 43672
5000000
r2 = 0,961
AUC
4000000
3000000 r = 0.9803
2000000
1000000
0
0 50 100 150 200
Konsentrasi (ppm)
Replikasi 2 Paracetamol
7000000
6000000 y = 35364x - 172074
R² = 0,9893
5000000 a = -172074
4000000 b = 35364
AUC
Replikasi 3 Paracetamol
6000000
3000000
r2= 0,9609
2000000 r = 0.9802
1000000
0
0 50 100 150 200
konsentrasi (ppm)
Pada baku parasetamol, persamaan regresi linier yang digunakan untuk menghitung
kadar adalah replikasi 2 karena memiliki nilai r = 0.9946 lebih mendekati nilai 1,
dibandingkan nilai r replikasi 1 dan 3.
4. Kurva Baku Ibuprofen
Replikasi 1 Replikasi 2 Replikasi 3
konsentrasi AUC konsentrasi AUC konsentrasi AUC
(ppm) (ppm) (ppm)
40 781714 40 723600 40 878381
60 1029707 60 1031771 60 1218188
70 1153765 70 1203848 70 1409751
80 1319124 80 1336962 80 1636694
90 1507308 90 1514881 90 1847692
100 1646629 100 1671321 100 1965876
Replikasi 1 Ibuprofen
1800000
1600000 y = 14654x + 165051
1400000 R² = 0,9928
a = 165051
1200000
b = 14654
1000000
r2 = 0,9928
AUC
800000
600000 r = 0.9946
400000
200000
0
0 20 40 60 80 100 120
konsentrasi (ppm)
Replikasi 2 Ibuprofen
1800000
1600000
1400000
1200000 a = 89239
1000000 b = 15789
AUC
800000
600000
y = 15789x + 89239 r2= 0,9993
R² = 0,9993
400000 r = 0.9996
200000
0
0 20 40 60 80 100 120
konsentrasi (ppm)
Replikasi 3 Ibuprofen
2500000
y = 18818x + 112783
2000000
R² = 0,9952
a = 112783
b = 18818
1500000
r2 = 0,9952
AUC
1000000
r = 0.9975
500000
0
0 20 40 60 80 100 120
konsentrasi (ppm)
Pada baku ibuprofen, persamaan regresi linier yang digunakan untuk menghitung kadar
adalah replikasi 2 karena memiliki nilai r = 0.9996 lebih mendekati nilai 1, dibandingkan
nilai r replikasi 1 dan 3.
5. Analisis kualitatif
(a)
(b)
(c)
a) Baku Parasetamol kosentrasi 140 ppm
b) Baku Ibuprofen konsentrasi 70 ppm
c) Sampel campuran Parasetamol dan Ibuprofen dalam tablet merk “x”
Dari gambar diatas, dapat dilihat waktu retensi (tR) masing-masing senyawa pada sampel
dan dibandingkan dengan waktu retensi baku yang ditunjukkan pada tabel berikut :
Senyawa tR baku tR sampel
Parasetamol 1.682 1.681
Ibuprofen 2.967 2.954
7. Penetapan Kadar Campuran Parasetamol dan Ibuprofen dalam Tablet Merk “X”
Replikasi Parasetamol Ibuprofen
ke- AUC Kadar % AUC Kadar %
(mg/tablet) Recovery (mg/tablet) Recovery
1 4990259 418.55 119.58 1180747 198.21 99.10
2 5080306 423.58 121.02 1254746 210.53 105.27
3 4932582 408.31 116.66 1200240 199.05 99.52
4 5143074 429.57 122.73 1201517 201.36 100.36
5 5075995 420.38 120.10 1189869 197.47 98.73
6 4638243 383.10 109.46 1209447 199.83 99.91
7 4990540 421.34 120.38 1201910 203.40 101.70
8 4970894 422.98 120.85 1172583 199.58 99.79
9 5016096 411.63 117.60 1231838 203.06 101.53
10 4922872 413.12 118.03 1198737 201.49 100.53
Rata-rata 415.26 118.64 Rata-rata 201.39 100.64
1) Replikasi 1
10 5
Faktor pengenceran = ( ) x ( )
3 0.44
= 3.33 x 11.36
= 37.82
Volume pembuatan = 10 ml
AUC Parasetamol = 5080306
AUC Ibuprofen = 1180747
- Parasetamol
y = bx + a
4990259 = 35364x + (- 172074)
4990259 + 172074 = 35364x
5,162,333 = 35364x
5162333
x = 35364
x = 145.977 ppm => 145.977 mg/L
Kadar = konsentrasi (ppm) x factor pengenceran
= 145.977 mg/10 ml x 37.82
= 55.208 mg/10ml
𝑘𝑎𝑑𝑎𝑟
Kandungan PCT 1 tab = x bobot rata-rata
𝑏𝑜𝑏𝑜𝑡 𝑠𝑎𝑚𝑝𝑒𝑙
55.208 𝑚𝑔
= x 754.56 mg
99.53 𝑚𝑔
= 418.544 mg/tab
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑃𝐶𝑇 𝑑𝑎𝑙𝑎𝑚 1 𝑡𝑎𝑏
%Recovery = x 100%
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑒𝑡𝑖𝑘𝑒𝑡
418.544 𝑚𝑔/𝑡𝑎𝑏
= x 100%
350 𝑚𝑔
= 119,584 %
- Ibuprofen
y = bx + a
1180747 = 15789x + 89239
1180747 – 89239 = 15789x
1091508 = 15789x
1091508
x = 15789
x = 69.130 ppm => 69.130 mg/L
Kadar = konsentrasi (ppm) x factor pengenceran
= 69.130 mg/10ml x 37.82
= 26.144 mg/10ml
𝑘𝑎𝑑𝑎𝑟
Kandungan Ibuprofen 1 tab = 𝑏𝑒𝑟𝑎𝑡 𝑝𝑒𝑛𝑖𝑚𝑏𝑎𝑛𝑔𝑎𝑛 x bobot rata-rata
26.144 𝑚𝑔
= x 754.56 mg
99.53 𝑚𝑔
= 198.20 mg/tab
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑖𝑏𝑢𝑝𝑟𝑜𝑓𝑒𝑛 𝑑𝑎𝑙𝑎𝑚 1 𝑡𝑎𝑏
%Recovery = x 100%
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑒𝑡𝑖𝑘𝑒𝑡
198.20 𝑚𝑔/𝑡𝑎𝑏
= x 100%
200 𝑚𝑔
= 99.1 %
2) Replikasi 2
AUC Parasetamol = 4990259
AUC Ibuprofen = 1254746
- Parasetamol
y = bx + a
5080306 = 35364x + (- 172074)
5080306 + 172074 = 35364x
5252380 = 35364x
5252380
x = 35364
= 423.589 mg/tab
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑃𝐶𝑇 𝑑𝑎𝑙𝑎𝑚 1 𝑡𝑎𝑏
%Recovery = x 100%
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑒𝑡𝑖𝑘𝑒𝑡
423.589 𝑚𝑔/𝑡𝑎𝑏
= x 100%
350 𝑚𝑔
= 121.025 %
- Ibuprofen
y = bx + a
1254746 = 15789x + 89239
1254746 – 89239 = 15789x
1165507 = 15789x
1165507
x = 15789
= 210.524 mg/tab
𝒌𝒂𝒏𝒅𝒖𝒏𝒈𝒂𝒏 𝑰𝒃𝒖𝒑𝒓𝒐𝒇𝒆𝒏 𝒅𝒂𝒍𝒂𝒎 𝟏 𝒕𝒂𝒃
%Recovery = x 100%
𝒌𝒂𝒏𝒅𝒖𝒏𝒈𝒂𝒏 𝒆𝒕𝒊𝒌𝒆𝒕
210.524 𝑚𝑔/𝑡𝑎𝑏
= x 100%
200 𝑚𝑔
= 105.262 %
3) Replikasi 3
AUC Parasetamol = 4932582
AUC Ibuprofen = 1200240
- Parasetamol
y = bx + a
4932582 = 35364x + (- 172074)
4932582 + 172074 = 35364x
5104656 = 35364x
5104656
x = 35364
𝑘𝑎𝑑𝑎𝑟
Kandungan PCT 1 tab = 𝑏𝑒𝑟𝑎𝑡 𝑝𝑒𝑛𝑖𝑚𝑏𝑎𝑛𝑔𝑎𝑛 x bobot rata-rata
54.591 𝑚𝑔
= x 754.56 mg
100,88 𝑚𝑔
= 408.328 mg/tab
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑃𝐶𝑇 𝑑𝑎𝑙𝑎𝑚 1 𝑡𝑎𝑏
%Recovery = x 100%
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑒𝑡𝑖𝑘𝑒𝑡
408.328 𝑚𝑔/𝑡𝑎𝑏
= x 100%
350 𝑚𝑔
= 116.665 %
- Ibuprofen
y = bx + a
1200240 = 15789x + 89239
1200240 – 89239 = 15789x
1111001 = 15789x
1111001
x = 15789
= 199.051 mg/tab
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝐼𝑏𝑢𝑝𝑟𝑜𝑓𝑒𝑛 𝑑𝑎𝑙𝑎𝑚 1 𝑡𝑎𝑏
%Recovery = x 100%
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑒𝑡𝑖𝑘𝑒𝑡
199.051 𝑚𝑔/𝑡𝑎𝑏
= x 100%
200 𝑚𝑔
= 99.525 %
4) Replikasi 4
AUC Parasetamol = 5143074
AUC Ibuprofen = 1201517
- Parasetamol
y = bx + a
5143074 = 35364x + (- 172074)
5143074 + 172074 = 35364x
5315148 = 35364x
5315148
X = 35364
= 429.594 mg/tab
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑃𝐶𝑇 𝑑𝑎𝑙𝑎𝑚 1 𝑡𝑎𝑏
%Recovery = x 100%
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑒𝑡𝑖𝑘𝑒𝑡
429.594 𝑚𝑔/𝑡𝑎𝑏
= x 100%
350 𝑚𝑔
= 122.741 %
- Ibuprofen
y = bx + a
1201517 = 15789x + 89239
1201517 – 89239 = 15789x
1112278 = 15789x
1112278
X = 15789
= 201.352 mg/tab
𝒌𝒂𝒏𝒅𝒖𝒏𝒈𝒂𝒏 𝑰𝒃𝒖𝒑𝒓𝒐𝒇𝒆𝒏 𝒅𝒂𝒍𝒂𝒎 𝟏 𝒕𝒂𝒃
%Recovery = x 100%
𝒌𝒂𝒏𝒅𝒖𝒏𝒈𝒂𝒏 𝒆𝒕𝒊𝒌𝒆𝒕
𝟐𝟎𝟏.𝟑𝟓𝟐 𝒎𝒈/𝒕𝒂𝒃
= x 100%
𝟐𝟎𝟎 𝒎𝒈
= 100.676 %
5) Replikasi 5
AUC Parasetamol = 5075995
AUC Ibuprofen = 1189869
- Paracetamol
y = bx + a
5075995 = 35364x + (- 172074)
5075995 + 172074 = 35364x
5248069 = 35364x
5248069
x = 35364
= 420.385 mg/tab
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑃𝐶𝑇 𝑑𝑎𝑙𝑎𝑚 1 𝑡𝑎𝑏
%Recovery = x 100%
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑒𝑡𝑖𝑘𝑒𝑡
420.385 𝑚𝑔/𝑡𝑎𝑏
= x 100%
350 𝑚𝑔
= 120.11 %
- Ibuprofen
y = bx + a
1189869 = 15789x + 89239
1189869 – 89239 = 15789x
1100630 = 15789x
1100630
x = 15789
= 197.463 mg/tab
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝐼𝑏𝑢𝑝𝑟𝑜𝑓𝑒𝑛 𝑑𝑎𝑙𝑎𝑚 1 𝑡𝑎𝑏
%Recovery = x 100%
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑒𝑡𝑖𝑘𝑒𝑡
197.463 𝑚𝑔/𝑡𝑎𝑏
= x 100%
200 𝑚𝑔
= 98.731 %
6) Replikasi 6
AUC Parasetamol = 4638243
AUC Ibuprofen = 1209447
- Paracetamol
y = bx + a
4638243 = 35364x + (- 172074)
4638243 + 172074 = 35364x
4810317 = 35364x
4810317
x = 35364
= 383.111 mg/tab
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑃𝐶𝑇 𝑑𝑎𝑙𝑎𝑚 1 𝑡𝑎𝑏
%Recovery = x 100%
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑒𝑡𝑖𝑘𝑒𝑡
383.111 𝑚𝑔/𝑡𝑎𝑏
= x 100%
350 𝑚𝑔
= 109.460 %
- Ibufrofen
y = bx + a
1209447 = 15789x + 89239
1209447 – 89239 = 15789x
1120208 = 15789x
1120208
x = 15789
= 199.825 mg/tab
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝐼𝑏𝑢𝑝𝑟𝑜𝑓𝑒𝑛 𝑑𝑎𝑙𝑎𝑚 1 𝑡𝑎𝑏
%Recovery = x 100%
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑒𝑡𝑖𝑘𝑒𝑡
199.825 𝑚𝑔/𝑡𝑎𝑏
= x 100%
200 𝑚𝑔
= 99.912 %
7) Replikasi 7
AUC Parasetamol = 4990540
AUC Ibuprofen = 1201910
- Paracetamol
y = bx + a
4990540 = 35364x + (- 172074)
4990540 + 172074 = 35364x
5162614 = 35364x
5162614
x = 35364
= 421.361 mg/tab
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑃𝐶𝑇 𝑑𝑎𝑙𝑎𝑚 1 𝑡𝑎𝑏
%Recovery = x 100%
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑒𝑡𝑖𝑘𝑒𝑡
421.361 𝑚𝑔/𝑡𝑎𝑏
= x 100%
350 𝑚𝑔
= 120.388 %
- Ibuprofen
y = bx + a
1201910 = 15789x + 89239
1201910 – 89239 = 15789x
1112671 = 15789x
1112671
x = 15789
= 203.403 mg/tab
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝐼𝑏𝑢𝑝𝑟𝑜𝑓𝑒𝑛 𝑑𝑎𝑙𝑎𝑚 1 𝑡𝑎𝑏
%Recovery = x 100%
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑒𝑡𝑖𝑘𝑒𝑡
203.403 𝑚𝑔/𝑡𝑎𝑏
= x 100%
200 𝑚𝑔
= 101.701 %
8) Replikasi 8
AUC Parasetamol = 4970894
AUC Ibuprofen = 1172583
- Paracetamol
y = bx + a
4970894 = 35364x + (- 172074)
4970894 + 172074 = 35364x
5142968 = 35364x
5142968
x = 35364
= 423.010 mg/tab
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑃𝐶𝑇 𝑑𝑎𝑙𝑎𝑚 1 𝑡𝑎𝑏
%Recovery = x 100%
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑒𝑡𝑖𝑘𝑒𝑡
423.010 𝑚𝑔/𝑡𝑎𝑏
= x 100%
350 𝑚𝑔
= 120.86 %
- Ibuprofen
y = bx + a
1172583 = 15789x + 89239
1172583 – 89239 = 15789x
1083344 = 15789x
1083344
X = 15789
= 199.572 mg/tab
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝐼𝑏𝑢𝑝𝑟𝑜𝑓𝑒𝑛 𝑑𝑎𝑙𝑎𝑚 1 𝑡𝑎𝑏
%Recovery = x 100%
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑒𝑡𝑖𝑘𝑒𝑡
199.572 𝑚𝑔/𝑡𝑎𝑏
= x 100%
200 𝑚𝑔
= 99.786 %
9) Replikasi 9
AUC Parasetamol = 5016096
AUC Ibuprofen = 1231838
- Paracetamol
y = bx + a
5016096 = 35364x + (- 172074)
5016096 + 172074 = 35364x
5188170 = 35364x
5188170
x = 35364
= 411.661 mg/tab
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑃𝐶𝑇 𝑑𝑎𝑙𝑎𝑚 1 𝑡𝑎𝑏
%Recovery = x 100%
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑒𝑡𝑖𝑘𝑒𝑡
411.661 𝑚𝑔/𝑡𝑎𝑏
= x 100%
350 𝑚𝑔
= 117.617 %
- Ibuprofen
y = bx + a
1231838 = 15789x + 89239
1231838 – 89239 = 15789x
1142599 = 15789x
1142599
x = 15789
= 203.056 mg/tab
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝐼𝑏𝑢𝑝𝑟𝑜𝑓𝑒𝑛 𝑑𝑎𝑙𝑎𝑚 1 𝑡𝑎𝑏
%Recovery = x 100%
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑒𝑡𝑖𝑘𝑒𝑡
203.056 𝑚𝑔/𝑡𝑎𝑏
= x 100%
200 𝑚𝑔
= 101.528 %
10) Replikasi 10
AUC Parasetamol = 4922872
AUC Ibuprofen = 1198737
- Paracetamol
y = bx + a
4922872 = 35364x + (- 172074)
4922872 + 172074 = 35364x
5094946 = 35364x
5094946
x = 35364
= 413.120 mg/tab
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑃𝐶𝑇 𝑑𝑎𝑙𝑎𝑚 1 𝑡𝑎𝑏
%Recovery = x 100%
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑒𝑡𝑖𝑘𝑒𝑡
413.120 𝑚𝑔/𝑡𝑎𝑏
= x 100%
350 𝑚𝑔
= 118.034 %
- Ibuprofen
y = bx + a
1198737 = 15789x + 89239
1198737 – 89239 = 15789x
1109498 = 15789x
1109498
x = 15789
= 201.499 mg/tab
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝐼𝑏𝑢𝑝𝑟𝑜𝑓𝑒𝑛 𝑑𝑎𝑙𝑎𝑚 1 𝑡𝑎𝑏
%Recovery = x 100%
𝑘𝑎𝑛𝑑𝑢𝑛𝑔𝑎𝑛 𝑒𝑡𝑖𝑘𝑒𝑡
201.499 𝑚𝑔/𝑡𝑎𝑏
= x 100%
200 𝑚𝑔
= 100.749 %
11) Rata-rata % recovery
𝑗𝑢𝑚𝑙𝑎ℎ 𝑡𝑜𝑡𝑎𝑙 𝑘𝑎𝑑𝑎𝑟 (𝑚𝑔/𝑡𝑎𝑏)
Rata-rata % Recovery Paracetamol = x 100%
10
1,186,484
= x 100%
10
= 118,6484 %
= 100,697 %