Disusi 10

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1.

Kosentrasi Larutan Baku


botol timbang + ekstrak = 13,3952 g
Botol timbang = 13,1435 g _
Bobot ektrak = 0,2517 g

Penimbangan dan konsentrasi Baku induk


Baku induk 1 = 0,2517 g ~251,7 mg
251 ,7 mg
= × 1000=5034 ppm
50 ml
Baku induk 2 = N1 x V1 = N2 x V2
5034 ppm x 4,0 ml = N2 x 10,0 ml
N2 = 2013,6 ppm
Konsentrasi baku kerja
BK 6 : N1 x V1 = N2 x V2
2013,6 ppm x 4,0 ml = N2 x 10,0 ml
N2 = 805,44 ppm
BK 5 : N1 x V1 = N2 x V2
2013,6 ppm x 3,0 ml = N2 x 10,0 ml
N2 = 604,08 ppm
BK 4 : N1 x V1 = N2 x V2
5034 ppm x 5,0 ml = N2 x 50,0 ml
N2 = 503,4 ppm
BK 3 : N1 x V1 = N2 x V2
805,44 ppm x 5,0 ml = N2 x 10,0 ml
N2 = 402,72 ppm
BK 2 : N1 x V1 = N2 x V2
604,08 ppm x 5,0 ml = N2 x 10,0 ml
N2 = 302,04 ppm
BK 1 : N1 x V1 = N2 x V2
402,72 ppm x 5,0 ml = N2 x 10,0 ml
N2 = 201,36 ppm
2. Perhitungan Konsentrasi Larutan Standar EPMS (dibuat 500 ppm untuk recovery)
botol timbang + ekstrak = 13,2013 g
Botol timbang = 13,1495 g _
Bobot ektrak = 0,0518 g ~ 51,8 mg
51, 8 mg
= × 1000=518 ppm
100 ml

3. Penimbangan sampel 20 mg → 0,02±10% (0,018 g -0,022 g )


 Sampel 1 → botol timbang + ekstrak = 12,8108 g
Botol timbang = 12,7895 g _
Bobot ektrak = 0,0213 g
 Sampel 2 → botol timbang + ekstrak = 12,6956 g
Botol timbang = 12,6737 g _
Bobot ektrak = 0,0219 g
 Sampel 3 → botol timbang + ekstrak = 13,1110 g
Botol timbang = 13,0906 g
Bobot ektrak = 0,0204 g

4. Penimbangan recovery 20 mg → 0,02±10% (0,018 g -0,022 g )


 Recovery 1 → botol timbang + ekstrak = 12,9669 g
Botol timbang = 12,9460 g _
Bobot ektrak = 0,0209 g
 Recovery 2 → botol timbang + ekstrak = 12,2763 g
Botol timbang = 12,2548 g _
Bobot ektrak = 0,0215 g
 Recovery 3 → botol timbang + ekstrak = 13,1123 g
Botol timbang = 13,0906 g _
Bobot ektrak = 0,0217 g
Tabel Konsentrasi dan Luas Area baku Kerja
Konsentrasi (ppm) Luas Area (AV) Sampel dan
BK Luas Area (AV)
Recovery
Teoritis Praktis (x) (y)

1 200 201,36 14455,3 S1 20429,0

2 300 302,04 25549,4 S2 21865,1

3 400 402,72 21885,7 S3 21704,4

4 500 503,40 22380,2 R1 18853,2

5 600 604,08 22750,5 R2 20104,8

6 800 805,44 25964,7 R3 19992,1

Regresi 6 BK
a : 16439,74
b : 12,18406
r hitung : 0,64 < r table (0,917)
1 sampel direject (BK2)
a : 12639,03
b : 17,576976 ~ 17,577
r hitung : 0,9324 < r table untuk 5 data

Perhitungan Konsentrasi kadar Sampel dan Recovery


a. S1
y = 17,577x + a
20429,0 = 17,577x + 12639,03
x = 443,19 ppm
b. S2
y = 17,577x + a
21865,1 = 17,577x + 12639,03
x = 524,89 ppm
c. S3
y = 17,577x + a
21704,4 = 17,577x + 12639,03
x = 515,75 ppm
d. R1
y = 17,577x + a
18853,2 = 17,577x + 12639,03
x = 353,54 ppm
e. R2
y = 17,577x + a
20104,8 = 17,577x + 12639,03
x = 424,75 ppm
f. R3
y = 17,577x + a
19992,1 = 17,577x + 12639,03
x = 418,335 ppm

Perhitungan sampel untuk penetapan kadar EPMS dalam ekstrak kering


% kadar cab-o-sil = bobot cab-o-sil/ bobot ekstrak kering x 100%
= 20 gram / 55,16 gram x 100% = 36,26%

Penimbangan sampel
Sampel 1 ektrak tanpa cab-o-sil = 21,3 mg - (36,26% x 21,3 mg) = 13,58 mg
Sampel 2 ektrak tanpa cab-o-sil = 21,9 mg - (36,26% x 21,9 mg) = 13,96 mg
Sampel 3 ektrak tanpa cab-o-sil = 20,4 mg - (36,26% x 20,4 mg) = 13,00 mg

Pengenceran 3 ml
3
Sampel 1 : x 443 , 19 ppm = 1329,57 ppm
1
3
Sampel 2 : x 524 , 89 ppm = 1574,67
1
3
Sampel 3 : x 515 , 75 ppm =1547,25 ppm
1
Bobot sampel dalam 5 ml
1329 ,57 mg
Sampel 1 : x 5 ml = 6,6479 mg
1000 ml
1574 , 67 mg
Sampel 2 : x 5 ml = 7,8734 mg
1000 ml
1547 ,25 mg
Sampel 3 : x 5 ml = 7,7363 mg
1000 ml

(%) EPMS dalam sampel


6,6479 mg
Sampel 1 : x 100 % = 48,95%
13 ,58 mg
7,8734 mg
Sampel 2 : x 100 % = 56,40%
13 , 96 mg
7,7363 mg
Sampel 3 : x 100 % = 59,51%
13 , 00 mg

Penentuan Presisi
48 , 95 %+ 56 , 40 %+ 59 ,51 %
Rata-rata : = 54,95%
3
SD : 5,4266
SD 5,4266
KV : x 100 % = x 100 % = 9,88%
rata−rata 54 , 95
Penimbangan recovery
Recovery 1 ektrak tanpa cab-o-sil = 20,9 mg - (36,26% x 20,9 mg) = 13,32 mg
Recovery 2 ektrak tanpa cab-o-sil = 21,5 mg - (36,26% x 21,5 mg) = 13,70 mg
Recovery 3 ektrak tanpa cab-o-sil = 21,7 mg - (36,26% x 21,7 mg) = 13,83 mg

Pengenceran 4 ml
4
Recovery 1 : x 353 , 54 ppm = 1414,16 ppm
1
4
Recovery 2 : x 424 , 75 ppm = 1699,00 ppm
1
4
Recovery 3 : x 418,335 ppm = 1673,34 ppm
1

Bobot recovery dalam 5 ml


1414 , 16 mg
Recovery 1 : x 5 ml = 7,0708 mg
1000 ml
1699 ,00 mg
Recovery 2 : x 5 ml = 8,4950 mg
1000 ml
1673 ,34 mg
Recovery 3 : x 5 ml = 8,3667 mg
1000 ml

(%) EPMS dalam recovery


7,0708 mg
Recovery 1 : x 100 % = 53,08%
13 , 32mg
8,4950 mg
Recovery 2 : x 100 % = 62,01%
13 , 70 mg
8,3667 mg
Recovery 3 : x 100 % = 60,50%
13 , 83 mg

453 , 08 %+ 62 ,01 % +60 ,50 %


Rata-rata : = 58,53%
3
Penentuan akurasi
 Ct : Kadar recovery dalam 5 ml
rata−rata sampel x bobot penimbangan recovery
 Cp :
100
Ct
 Recovery : x 100 %
Cp+ Cst

Ct Cp Cst recovery

54 , 95 x 13 , 32 7,0708
7,0708 mg Cp1 = =7 , 32 0,518 R1 = x 100 %=90 ,21 %
100 7 ,32+ 0,518

54 , 95 x 13 , 70 8,4950
8,4950 mg Cp2 = =7 , 53 0,518 R2 = x 100 %=105 ,55 %
100 7 ,53+ 0,518

54 , 95 x 13 , 83 8,3667
8,3667 mg Cp3 = =7 , 60 0,518 R3 = x 100 %=103 , 06 %
100 7 , 60+0,518

90 , 21% +105 , 55 %+103 , 06 %


Rata-rata : = 99,61%
3

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