Identifikasi dan penetapan kadar zat warna merah dalam dawet yang dijual di sepanjang jalan “X” secara KLT Densitometri - Widya Mandala Catholic University Surabaya Repository
Lampiran I
Perhitungan Linieritas Rhodamin B
No
1.
x:z
Area
y
L: totolan (J.tg)
X
0,0618
X.Y
y:z
471,5
3,8192 . 10"3
29,1387
222312,25
3
2.
0,0824
583,5
6' 7898 . 10"
48,0804
340472,25
3.
0,1236
758,6
15,2770 . 1o·3
93,7630
575473,96
4.
0,1442
855,9
20,7936 . 10"3
123,4208
732564,81
5.
0,1648
972,0
27,1590 . 10"3
160,1856
944784,00
6.
0,1854
1049,5
34,3732 . 10"3
194,5773
1101450,25
L:
0,7622
4691
108,2118. 10"-'
649,1658
3917057,52
n.L:(X.Y)-(L:X}(L:Y)
r
6.649,1658 -(0,7622}(4691)
~(6
.to8,2tt8 .10-3
-
(o,1622y )(6. 3917057,52- (4691Y)
3894,9948-3575,4802
~(649,2708
.10" 3 -580,9488 .10"3 )(23502345, 12- 22005481)
319,5146
~=-r
3
~(68,32.10"
319,5164
)(1496864,12)
.Jt02268,7504
319,5146
319,7949
= 0,9991
b
= n.L:(X.Y)-(L:xXL:Y)
n.L:X 2 -(L:xY
= 6. 649,1658- (0,7622)(4691)
6.to8,2118.10-3 -(o,7622Y
3894,9948-3575,4802
= (6 .108,2118 .10- 3 ) - (o, 7662
y
73
319,5146
3
= (649,2708 .10" ) - (580,9488 .10" 3 )
319,5146
68 ' 322 . 10-3
=
4676,5991
:EY- b .:EX
a
n
=
4691- (4676,5991. 0,7622)
6
=
4691-3564,5038
6
1126,4962
6
=
187,7494
74
•
Koefisien variasi dari fungsi
No
~
1.
totolan (IJ.g)
X
0,0618
Area
y
yi = bx +a
lyi- Yi
471,5
476,7632
27,7013
2
2.
0,0824
583,5
573,1012
108,1350
3.
0,1236
758,6
765,7771
51,5108
4.
0,1442
855,9
862,1150
38,6262
5.
0,1648
972,0
958,4529
183,5239
6.
0,1854
1049,5
1054,7909
27,9936
2:
0,7662
4691
X
Sy
=
=0,1277
YY
~(yi-
n-2
437,4908
6-2
=
10,4581
Sxo - Sy
b
10,4581
4676,5991
= 2,2363 . 10-3
Vxo = S_:o . 100%
X
2,2363.100,1277
= 1,75%
3
.
%
100
(< 2% ~
memenuhi syarat)
75
437,4908
•
Pembuktian Xp
No
x'J.
Area
1.
L totolan (!lg)
X
0,0618
471,5
3,8192. 10-j
2.
0,0824
583,5
3.
0,1236
758,6
6' 7898 . 10"3
15,2770. 10"3
4.
0,1442
855,9
20,7936. 10"3
5.
0,1648
972,0
27,1590 . 10"3
6.
0,1854
1049,5
34,3732 . 1o·3
L
0,7662
4691
108,2118. 10-.1
X
Qxx
=
y
-
= 0,1277
2
1
LX - - (Lx)
y = 781,8333
2
n
= 108,2118 . 10"3 - _!_ (0, 7662)2
6
= 108,2118. 10"3 - 97,8437. 10"3
= 10,3681 . 10"3
Yp
R
~a+Sy.t"'·
=
187 74 94 + 10 4581 . 2 132.
' '
'
'
.!.+ 1 +
=
187,7494 + 10,4581 . 2,132. 1,6551
=
224,6526
6
76
(o,1277 Y3
10,3681.10-
Xp
X
=
2 . Sxo . ttabel
=
2 . 2,2363 .
w-3 . 2,132 .
=
2 . 2,2363 .
w-3 . 2,132 . 1,5924
=
0,0152 f.!g
=
0,0618 f.!g
.
(224,6526 - 781,8333
y
(4676,5991Y .10,3681.10- 3
Xp < X ....._, memenuhi syarat
PE .~ t>USTACAAN
UoiYenJtaa Katol ilr Wiclp Muadala
iURABAYA
77
1
+ 1 +6
Lampiran 2
Perhitungan Homogenitas
Area Konsentrasi
Terkecil
Area Konsentrasi
Terbesar
470,4
1070,1
472,1
1069,9
472,5
1069,8
471,9
1067,9
471,5
1068,3
469,9
1069,4
472,3
1067,8
469,5
1069,5
471,7
1070,3
471,4
1068,5
SL = 1,0358
SN = 0,9384
PW= SN2
se
0,9384 2
1,0358 2
0,8806
1,0729
=--
=
0,8208
78
Lampiran 3
Perhitungan LOD dan LOQ
Area
Jumlah totolan (J.lg)
-
Blangko
Sampel
0,0041
-
0,0062
-
0,0082
-
0,0103
-
0,0206
-
0,0412
323,6
0,0618
471,5
0,0824
583,5
0,1030
584,4
0,1236
758,6
0,1442
855,9
0,1648
972,0
0,1854
1049,5
0,2060
-
Tidak dapat dihitung karena pada blangko tidak ada serapan sama sekali sehingga
LOD ditetapkan 0,0412 J.lg
LOQ ditetapkan 0,0618 J.tg
79
Lampiran4
Perhitungan Akurasi dan Presisi Rhodamin B
Kurva baku
L totolan (j..tg)
Area
0,0618
473,5
0,1236
762,8
0,1442
856,8
0,1648
975,3
0,1854
1052,3
y = 4743,039x + 179,2764
r = 0,9993
I. 103,0 mg ad 25 ml
Pipet 4 ml
~
_.±_
25
x 103 = 16,48 mg
Berat bersih dawet = 57,15 g
Kadar zat warna dalam dawet =
16 48 w- 3
' ·
x 100% = 0,029%
57,15
%recovery
Dawet ditimbang
Area
j..tg sampel
5,1251
1557,3
0,2905
Jumlah (mg)
Diperoleh
Dibuat
1,4779
1,4525
4,9424
1514,6
0,2815
1,4252
1,4075
98,76
5,0103
1536,4
0,2861
1,4448
1,4305
99,01
5,0190
1529,3
0,2846
1,4473
1,4230
98,32
5,1858
1571,8
0,2936
1,4954
1,4680
98,17
98,28
% rec. rata-rata= 98,51
Contoh perhitungan :
Area
= 1557,3
~
sampel = 0,2905 j..tg I 5 j..tl
= 1452,5 j..tg I 25 ml
=
1,4525 mg I 25 ml
80
Dalam 5,1251 g dawet terkandung zat pewarna sebanyak:
5 1251
'
x 16 48
5715
'
'
% recovery =
= 1 4779 m
'
g
1,4525
x 100% = 98,28%
1,4779
Jumlah diperoleh
lx-
~12
X
1,4525
2,6244. 10-4
1,4075
8,2944. 10-4
1,4305
3' 3640 . 10-5
1' 7689 . 10-4
1' 0049 . 10-3
1,4230
1,4680
-
L = 2,3073 . 10-3
1,4363
X =
2,3073.10-3
5-1
=
KV
=
0,0240
S_? . 100%
X
=
0,0240 . 100%
1,4363
=
1,67% (< 2%
~
memenuhi syarat)
81
II. 103,0 mg ad 25 ml
Pipet 2 ml
~
~
25
x 103 = 8,24 mg
Berat bersih dawet = 59,14 g
8 24 w- 3
Kadar zat warna dalam dawet = ' ·
x 100% = 0,014%
59,14
Jumlah (mg)
Dibuat
Diperoleh
%recovery
Dawet ditimbang
Area
J...Lg sampel
5,1819
857,8
0,1431
0,7220
0,7155
99,10
5,1069
847,3
0,1408
0,7115
0,7040
98,95
5,2149
861,7
0,1439
0,7266
0,7195
99,02
5,1503
852,4
0,1419
0,7176
0,7095
98,87
5,3283
874,9
0,1467
0,7424
0,7335
98,80
% rec. rata-rata= 98,93
Contoh perhitungan :
Area
= 857,8
~
sampel = 0,1431 J...Lg I 5 J.. Ll
= 715,5 J...Lg I 25 ml
= 0,7155 mg I 25 ml
Dalam 5, 1819 g dawet terkandung zat pewarna sebanyak :
5 1819
x824=07220m
'
5914
'
'
g
'
%recovery=
0 7155
'
x 100% = 99,10%
0,7220
82
Jumlah diperoleh
lx-
~12
X
0,7155
0,7040
' .
1' 5376 . 10-4
0,7195
9,61 . 10-6
0,7095
4' 761 . 10-5
2, 9241 . 104
0,7335
X
8 1 10-7
= 0,7164
L = 5' 042 . 10-4
5' 042 .10-4
5-1
=
KV
=
0,0112
S_? . 100%
X
= 0,0112 . 100%
0,7164
= 1,56% (< 2% ~
memenuhi syarat)
83
Lampiran 5
Perhitungan Penetapan Kadar Rhodamin B dalam Sampel
Kurva baku
L, totolan (!!g)
Area
X
y
0,0618
473,5
0,1236
762,8
0,1442
856,8
0,1648
975,3
0,1854
1052,3
Sampel
&
Replikasi
II 1
2
3
4
r
=
0,9993
Oawet yang
ditimbang
(g)
5,0768
5,1036
5,3021
5,2137
0,016
0,015
0,015
0,017
10"6
10"6
10"6
10"6
5,6850
5,1352
5,2517
5,3814
0,013
0,014
0,013
0,013
817,0.
882,5.
857,0.
879,0.
10"6
10"6
10"6
10"6
5,8357
5,8856
5,7143
5,8614
0,014
0,015
0,015
0,015
0,1169
0,1317
0,1141
0,1138
584,5.
658,5.
570,5.
569,0.
10"6
10"6
10"6
10"6
5,3123
5,4899
5,1853
5,1714
0,011
0,012
0,011
0,011
0,1465
0,1516
0,1487
0,1525
732,5.
758,0.
743,5.
762,5.
10"6
10"6
10"6
10"6
5,2312
5,8301
5,3133
5,8671
0,014
0,013
0,014
0,013
Area
2:totolan
(J.tg/5 J.tll
950,0
905,4
933,9
1020,2
0,1625
0,1531
0,1591
0,1773
Zat warna
dalam dawet
(g/25ml)
812,5. 10"6
765,5- 10"6
795,5. 10"6
886,5. 10"6
1
2
3
4
880,3
861,3
826,7
842,8
0,1478
0,1438
0,1365
0,1399
739,0.
719,0.
682,5.
699,5.
XI 1
2
3
4
954,3
1016,4
992,2
1013,1
0,1634
0,1765
0,1714
0,1758
Xlll1
2
3
4
733,7
803,9
720,5
719,0
XVI1
2
3
4
874,1
898,3
884,6
902,6
v
y = 4743,039x + 179,2764
84
Kadar
(%)
Kadar
ratarata
SO kadar
%rec
sesungguhnya
0,016
9,5743. 10"4
0,016%
0,013
5,00.10"4
0,013%
0,015
5,00.10"4
0,015%
0,011
5,00.10"4
0,011%
0,014
5,7735.10"4
0,014%
Contoh perhitungan :
Area
=
950
~
sampel
=
0,1625 J.tg I 5 J.tl
= 812,5. 10-6 g/ 25 ml
Kadar=
6
812 5
' .l05,0768
.
100% = 0 016%
'
% recovery sesungguhnya =
100
kadar rata-rata. - - - - - - - - - - - - - - - - - - % recovery rata - rata dengan kadar zat warna 0, 014%
=0016. ~
'
98,95
= 0,016
%recovery rata-rata dengan kadar zat warna dawet yang dibuat 0,014%
= 99,10 + 98,95 + 99,02 + 98,87 + 98,80
5
= 98,95
85
Lampiran 6
Area Linieritas Rhodamin B
1
2
/
3
4
4
/
3
5
/
6
6
7
8
9
7
8
9
lEI
/
This
This
5? .1
5?.0
This
56.9
57.2
58.121
58.8
This
track was
track was
0.1
0.1
tracl< was
0.1
0.1
0,2
0.2
tracl< was
Substance: 1
P .deu .range:
CU [~]
n
SI
t1D
area: .ean
No result for this substance available,
CAMAG SOFTUAHE
86
(c)
5~
1996
SCANNEH 3:
020301
Lampiran 7
Area Homogenitas Rhodamin B
SPICT~UM
Uld~a
nandala
tntesrat Iqn MbdOriiluill Speetrurt
:n: LANI9
Method
Scan
TLCAIPTLC-Eualuation (CAtS Ui.M. ~:81M
Substance: 1
Di.:nsion:
track Sl
rm
cal i
area
X(calc)
1
2
3
1
2
3
4
4
5
6
7
a
9
18
11
12
13
14
15
16
17
1a
19
5
6
7
a
9
a
b
c
d
e
r
g
h
1
J
SPECT~UM
nethqd
1
End
/ Sc3 U1.13. ~:8Z31)
p.d.eu.range:
Jig
57 . 9
8 . 1 4 79.4
59.a
8.1
472.1
59 . 3
8 . 1 412. 5 .
59 . 4
8 •1
47 t. 9
59.9
8.1
471.5
59.9
8.1
469.9
59.7
8,2
472.3
59 . 4
8 .2
469 . 5
59 . 4
8 .2
4 7 t. 1
5a.a
471.4
69.2
1978. 1
69.3
1969.9
69,8
1969.a
69.8
1967.9
6a.a
1e6a.3
69.8
1869,4
69.4
1867.a
68,6
1869,5
63.4
1878.3
U4,B4 S/N:84B1ABB1
CAMAG SOFTUABE Ccl 1996
~
5
9:34
HE£P
f.t.J
YJ
SCANNER 3:
:n: tANI ,_
Uld~a
nandala
Scan Integrat Ign IMiuiillehl Spee$run
21/JUL/2888 9:4a
Data End
HlfP
YJ
(CAts Uot.M. SAI:M81M81 / Sc3 U1.13. SAI:eze381)
TLCAIPTLC-Eualuatian
Substance: 1
traclc Sl
tm
cali
1
21/JUL/2888
Data
64,7
Substance: 1
SI
tm
8.2
area
P!J
Dl-=nslon:
X(calc)
p.cleu.range:
186a.5
P .cleu.range:
area: .ean
CU (:.'.]
No result for this substance available,
n
5 :.'.
5
~
t.t.J
828391
Lampiran 8
Area LOD dan LOQ Rhodamin B
SPECTRUM
:M: LANU8
Uidya r~andl
21/JUL/2888 9:34
Method Scan Integratlgn liliddliildli Spectrun Data End
H&tP
nCAtPTLC-Eualuation (CATS U1.e1. SJ'ft:8181A881 / Sc3 U1.13, s..-tt:eze39U
Y]
Substance : 1
DI .ens ion:
pg
p.deu.range:
5 "Track Sl
I1D
cal i
area
XCcalc)
No peak detected.
1
1
2
2
No peak detected,
3
3
No peak detected,
4
4
No peak detected,
5
5
~peak
detected,
6
6
No peak detected,
7
7
·No peak detected.
8
8
No peak detected.
9
9
No peak detected,
18
a
No peak detected.
11
b
59.2
323,6
12
c
59.3
471.5
13
d
59.8
583,5
14
e
59.8
584:.4
15
f
58.8
758,6
16
g
59.8
855.9
17
h
59.4
972.8
18
68.6
1849.5
19
j
No peak detected.
t•J
Substance: 1
Sl
11D
area:
-=an
P.deu.range:
5 "CU [X]
n
CAMAG SOFTUARE Cc) 1996
88
SCANNER 3:
828381
Lampiran 9
Area Akurasi dan Presisi Rhodamin B
SPECTRUM
:M: LANlll
Uid~a
nandala
Method Scan Integration libb,)Jiiiuj.l Spectrun
22-'JUL/2eee
Data
End
9:18
HEkf
tLCAtPnc-Eualuation (CATS IH.&i, SA1:&4e1Ae81 / Sc3 U1.13, SAI:8283e1l t•Jt•l
Di..ension:
Jig
p.deu.range:
5 %
Substance: 1
X(calc)
cali
track SI
area
tm
57.e
1
1
e. 1 473.5
2
2
56.9
e .1 762.8
3
3
57.2
e .1 856.8
4
1
58.e
e .1 975.3
58,8
5
5
e .1 1EI5Z.3
6
63.0
a
1557.3
7
63.0
1514.6
b
62.7
a c
1536.4
62.7
9
d
1529.3
lEI
e
62.6
1571.8
f
62.6
11
857.8
g
12
62.4
847.3
h
86_1,7
13
62.6
14
63.1
852.4
j
15
63.4
871.9
Substance: 1
P.deu.range:
5%
area: aean
CU [%]
n
tm
SI
62.6
••••
••
e
a
b
62.6
••••
••
e
c
62.4
159,3te ng
••
1
62.6
••••
••
e
d
U4.B4 S/N:EI4B1ABB1
CAMAG SOFTUARE Ccl 1996
89
SCANNER 3:
B2e3e1
Lampiran 10
Area Kadar Sampel
SPECTRUM
22/JUL/2888 9:48
Data End
H&EP
TLCAiPTLC-Eualuation (CATS Ui.&i. SAt:&i81Mel / Sc3 U1.13. SAt:828381)
p.dcu.rangc:
Di..:nsion:
pg
Substance: 1
5%
X(calc)
nD
cali area
Traclc Sl
57,8
1
473.5
1
8.1
56.9
2·
8. 1 762.8
2
57.2
3
856.8
3
8.1
58.8
4
4
8.1
975.3
58.8
5
5
8.1 1852,3
a
63.8
958.8
6
b
995,4
7
63.8
c
62.7
933.9
8
d
62.7
1829.2
9
e
62.6
18
889.3
f
62.6
11
861.3
g
826,7
62.4
12
h
62.6
842.8
13
Method
:M: LANI12
Sc:an
Substance: 1
Sl
a
b
c
d
nandala
Uid~:a
Integrat !on lldn1ijiii.hi Spec:trurt
P .dcu .range:
5%
[%]
n
62,6
8
****
**
62.6
8
****
**
62,4
59.318 ng
1
**
62,6
8
****
**
U4.84 S/N:8481A881
CAMAG SOFTUAHE Cc) 1996
nD
area: .:an
t•J •J
cu
90
SCANNEH 3:
828381
S?!CTRUn
:n: LANI13
22/JUL/2eea 9:34
Dda End
HifP
nCAIPTLC-Eualuation (CATS Ui.EH. SA1:9191.Aee1 / Sc3 U1.13. SAt:9Z93ell t•J ,.J
p.dcu.rangc:
5%
Substdna:: 1
Di.:nsion:
Jig
X(calc)
cali
Track SI
nD
area
473,5
1
1
57.a
a. 1
2
2
a. 1
762.8
56,9
e. 1
3
57.2
856.8
3
4
a. 1
4
975.3
58.8
5
a .1 tesz.3
5
58.8
59,9
954.3
6
a
59,7
1816,4
7
b
59,4
c
8
992.2
d
59.4
9
1a 13. 1
e
58,8
te
733.7
f
11
59.2
8a3.9
g
59,3
12
729.5
h
59,8
13
7·19. a
14
59.8
874.1
j
58,9
15
998.3
k
16
59.a
884,6
59,4
17
1
992.6
Method
Scan
Substance: 1
SI
tm
Uidya "andala
Integrat jon lltl1b.Jiiii1Uli Spectrul"'
P .deu.range:
area:
-=an
CU [;d
5
:1.
n
CAMAG SOFTUAFIE
91
Cc)
't996
SCANNEFI 3:
a2a3a1
Lampiran 11
NATIONAL OUAUTY CONTROL LABORATORY OF
ORUG AND FOOD
PUSAT PEMEAIKSAAN 08AT DAN MAKANAN
Di
Perhitungan Linieritas Rhodamin B
No
1.
x:z
Area
y
L: totolan (J.tg)
X
0,0618
X.Y
y:z
471,5
3,8192 . 10"3
29,1387
222312,25
3
2.
0,0824
583,5
6' 7898 . 10"
48,0804
340472,25
3.
0,1236
758,6
15,2770 . 1o·3
93,7630
575473,96
4.
0,1442
855,9
20,7936 . 10"3
123,4208
732564,81
5.
0,1648
972,0
27,1590 . 10"3
160,1856
944784,00
6.
0,1854
1049,5
34,3732 . 10"3
194,5773
1101450,25
L:
0,7622
4691
108,2118. 10"-'
649,1658
3917057,52
n.L:(X.Y)-(L:X}(L:Y)
r
6.649,1658 -(0,7622}(4691)
~(6
.to8,2tt8 .10-3
-
(o,1622y )(6. 3917057,52- (4691Y)
3894,9948-3575,4802
~(649,2708
.10" 3 -580,9488 .10"3 )(23502345, 12- 22005481)
319,5146
~=-r
3
~(68,32.10"
319,5164
)(1496864,12)
.Jt02268,7504
319,5146
319,7949
= 0,9991
b
= n.L:(X.Y)-(L:xXL:Y)
n.L:X 2 -(L:xY
= 6. 649,1658- (0,7622)(4691)
6.to8,2118.10-3 -(o,7622Y
3894,9948-3575,4802
= (6 .108,2118 .10- 3 ) - (o, 7662
y
73
319,5146
3
= (649,2708 .10" ) - (580,9488 .10" 3 )
319,5146
68 ' 322 . 10-3
=
4676,5991
:EY- b .:EX
a
n
=
4691- (4676,5991. 0,7622)
6
=
4691-3564,5038
6
1126,4962
6
=
187,7494
74
•
Koefisien variasi dari fungsi
No
~
1.
totolan (IJ.g)
X
0,0618
Area
y
yi = bx +a
lyi- Yi
471,5
476,7632
27,7013
2
2.
0,0824
583,5
573,1012
108,1350
3.
0,1236
758,6
765,7771
51,5108
4.
0,1442
855,9
862,1150
38,6262
5.
0,1648
972,0
958,4529
183,5239
6.
0,1854
1049,5
1054,7909
27,9936
2:
0,7662
4691
X
Sy
=
=0,1277
YY
~(yi-
n-2
437,4908
6-2
=
10,4581
Sxo - Sy
b
10,4581
4676,5991
= 2,2363 . 10-3
Vxo = S_:o . 100%
X
2,2363.100,1277
= 1,75%
3
.
%
100
(< 2% ~
memenuhi syarat)
75
437,4908
•
Pembuktian Xp
No
x'J.
Area
1.
L totolan (!lg)
X
0,0618
471,5
3,8192. 10-j
2.
0,0824
583,5
3.
0,1236
758,6
6' 7898 . 10"3
15,2770. 10"3
4.
0,1442
855,9
20,7936. 10"3
5.
0,1648
972,0
27,1590 . 10"3
6.
0,1854
1049,5
34,3732 . 1o·3
L
0,7662
4691
108,2118. 10-.1
X
Qxx
=
y
-
= 0,1277
2
1
LX - - (Lx)
y = 781,8333
2
n
= 108,2118 . 10"3 - _!_ (0, 7662)2
6
= 108,2118. 10"3 - 97,8437. 10"3
= 10,3681 . 10"3
Yp
R
~a+Sy.t"'·
=
187 74 94 + 10 4581 . 2 132.
' '
'
'
.!.+ 1 +
=
187,7494 + 10,4581 . 2,132. 1,6551
=
224,6526
6
76
(o,1277 Y3
10,3681.10-
Xp
X
=
2 . Sxo . ttabel
=
2 . 2,2363 .
w-3 . 2,132 .
=
2 . 2,2363 .
w-3 . 2,132 . 1,5924
=
0,0152 f.!g
=
0,0618 f.!g
.
(224,6526 - 781,8333
y
(4676,5991Y .10,3681.10- 3
Xp < X ....._, memenuhi syarat
PE .~ t>USTACAAN
UoiYenJtaa Katol ilr Wiclp Muadala
iURABAYA
77
1
+ 1 +6
Lampiran 2
Perhitungan Homogenitas
Area Konsentrasi
Terkecil
Area Konsentrasi
Terbesar
470,4
1070,1
472,1
1069,9
472,5
1069,8
471,9
1067,9
471,5
1068,3
469,9
1069,4
472,3
1067,8
469,5
1069,5
471,7
1070,3
471,4
1068,5
SL = 1,0358
SN = 0,9384
PW= SN2
se
0,9384 2
1,0358 2
0,8806
1,0729
=--
=
0,8208
78
Lampiran 3
Perhitungan LOD dan LOQ
Area
Jumlah totolan (J.lg)
-
Blangko
Sampel
0,0041
-
0,0062
-
0,0082
-
0,0103
-
0,0206
-
0,0412
323,6
0,0618
471,5
0,0824
583,5
0,1030
584,4
0,1236
758,6
0,1442
855,9
0,1648
972,0
0,1854
1049,5
0,2060
-
Tidak dapat dihitung karena pada blangko tidak ada serapan sama sekali sehingga
LOD ditetapkan 0,0412 J.lg
LOQ ditetapkan 0,0618 J.tg
79
Lampiran4
Perhitungan Akurasi dan Presisi Rhodamin B
Kurva baku
L totolan (j..tg)
Area
0,0618
473,5
0,1236
762,8
0,1442
856,8
0,1648
975,3
0,1854
1052,3
y = 4743,039x + 179,2764
r = 0,9993
I. 103,0 mg ad 25 ml
Pipet 4 ml
~
_.±_
25
x 103 = 16,48 mg
Berat bersih dawet = 57,15 g
Kadar zat warna dalam dawet =
16 48 w- 3
' ·
x 100% = 0,029%
57,15
%recovery
Dawet ditimbang
Area
j..tg sampel
5,1251
1557,3
0,2905
Jumlah (mg)
Diperoleh
Dibuat
1,4779
1,4525
4,9424
1514,6
0,2815
1,4252
1,4075
98,76
5,0103
1536,4
0,2861
1,4448
1,4305
99,01
5,0190
1529,3
0,2846
1,4473
1,4230
98,32
5,1858
1571,8
0,2936
1,4954
1,4680
98,17
98,28
% rec. rata-rata= 98,51
Contoh perhitungan :
Area
= 1557,3
~
sampel = 0,2905 j..tg I 5 j..tl
= 1452,5 j..tg I 25 ml
=
1,4525 mg I 25 ml
80
Dalam 5,1251 g dawet terkandung zat pewarna sebanyak:
5 1251
'
x 16 48
5715
'
'
% recovery =
= 1 4779 m
'
g
1,4525
x 100% = 98,28%
1,4779
Jumlah diperoleh
lx-
~12
X
1,4525
2,6244. 10-4
1,4075
8,2944. 10-4
1,4305
3' 3640 . 10-5
1' 7689 . 10-4
1' 0049 . 10-3
1,4230
1,4680
-
L = 2,3073 . 10-3
1,4363
X =
2,3073.10-3
5-1
=
KV
=
0,0240
S_? . 100%
X
=
0,0240 . 100%
1,4363
=
1,67% (< 2%
~
memenuhi syarat)
81
II. 103,0 mg ad 25 ml
Pipet 2 ml
~
~
25
x 103 = 8,24 mg
Berat bersih dawet = 59,14 g
8 24 w- 3
Kadar zat warna dalam dawet = ' ·
x 100% = 0,014%
59,14
Jumlah (mg)
Dibuat
Diperoleh
%recovery
Dawet ditimbang
Area
J...Lg sampel
5,1819
857,8
0,1431
0,7220
0,7155
99,10
5,1069
847,3
0,1408
0,7115
0,7040
98,95
5,2149
861,7
0,1439
0,7266
0,7195
99,02
5,1503
852,4
0,1419
0,7176
0,7095
98,87
5,3283
874,9
0,1467
0,7424
0,7335
98,80
% rec. rata-rata= 98,93
Contoh perhitungan :
Area
= 857,8
~
sampel = 0,1431 J...Lg I 5 J.. Ll
= 715,5 J...Lg I 25 ml
= 0,7155 mg I 25 ml
Dalam 5, 1819 g dawet terkandung zat pewarna sebanyak :
5 1819
x824=07220m
'
5914
'
'
g
'
%recovery=
0 7155
'
x 100% = 99,10%
0,7220
82
Jumlah diperoleh
lx-
~12
X
0,7155
0,7040
' .
1' 5376 . 10-4
0,7195
9,61 . 10-6
0,7095
4' 761 . 10-5
2, 9241 . 104
0,7335
X
8 1 10-7
= 0,7164
L = 5' 042 . 10-4
5' 042 .10-4
5-1
=
KV
=
0,0112
S_? . 100%
X
= 0,0112 . 100%
0,7164
= 1,56% (< 2% ~
memenuhi syarat)
83
Lampiran 5
Perhitungan Penetapan Kadar Rhodamin B dalam Sampel
Kurva baku
L, totolan (!!g)
Area
X
y
0,0618
473,5
0,1236
762,8
0,1442
856,8
0,1648
975,3
0,1854
1052,3
Sampel
&
Replikasi
II 1
2
3
4
r
=
0,9993
Oawet yang
ditimbang
(g)
5,0768
5,1036
5,3021
5,2137
0,016
0,015
0,015
0,017
10"6
10"6
10"6
10"6
5,6850
5,1352
5,2517
5,3814
0,013
0,014
0,013
0,013
817,0.
882,5.
857,0.
879,0.
10"6
10"6
10"6
10"6
5,8357
5,8856
5,7143
5,8614
0,014
0,015
0,015
0,015
0,1169
0,1317
0,1141
0,1138
584,5.
658,5.
570,5.
569,0.
10"6
10"6
10"6
10"6
5,3123
5,4899
5,1853
5,1714
0,011
0,012
0,011
0,011
0,1465
0,1516
0,1487
0,1525
732,5.
758,0.
743,5.
762,5.
10"6
10"6
10"6
10"6
5,2312
5,8301
5,3133
5,8671
0,014
0,013
0,014
0,013
Area
2:totolan
(J.tg/5 J.tll
950,0
905,4
933,9
1020,2
0,1625
0,1531
0,1591
0,1773
Zat warna
dalam dawet
(g/25ml)
812,5. 10"6
765,5- 10"6
795,5. 10"6
886,5. 10"6
1
2
3
4
880,3
861,3
826,7
842,8
0,1478
0,1438
0,1365
0,1399
739,0.
719,0.
682,5.
699,5.
XI 1
2
3
4
954,3
1016,4
992,2
1013,1
0,1634
0,1765
0,1714
0,1758
Xlll1
2
3
4
733,7
803,9
720,5
719,0
XVI1
2
3
4
874,1
898,3
884,6
902,6
v
y = 4743,039x + 179,2764
84
Kadar
(%)
Kadar
ratarata
SO kadar
%rec
sesungguhnya
0,016
9,5743. 10"4
0,016%
0,013
5,00.10"4
0,013%
0,015
5,00.10"4
0,015%
0,011
5,00.10"4
0,011%
0,014
5,7735.10"4
0,014%
Contoh perhitungan :
Area
=
950
~
sampel
=
0,1625 J.tg I 5 J.tl
= 812,5. 10-6 g/ 25 ml
Kadar=
6
812 5
' .l05,0768
.
100% = 0 016%
'
% recovery sesungguhnya =
100
kadar rata-rata. - - - - - - - - - - - - - - - - - - % recovery rata - rata dengan kadar zat warna 0, 014%
=0016. ~
'
98,95
= 0,016
%recovery rata-rata dengan kadar zat warna dawet yang dibuat 0,014%
= 99,10 + 98,95 + 99,02 + 98,87 + 98,80
5
= 98,95
85
Lampiran 6
Area Linieritas Rhodamin B
1
2
/
3
4
4
/
3
5
/
6
6
7
8
9
7
8
9
lEI
/
This
This
5? .1
5?.0
This
56.9
57.2
58.121
58.8
This
track was
track was
0.1
0.1
tracl< was
0.1
0.1
0,2
0.2
tracl< was
Substance: 1
P .deu .range:
CU [~]
n
SI
t1D
area: .ean
No result for this substance available,
CAMAG SOFTUAHE
86
(c)
5~
1996
SCANNEH 3:
020301
Lampiran 7
Area Homogenitas Rhodamin B
SPICT~UM
Uld~a
nandala
tntesrat Iqn MbdOriiluill Speetrurt
:n: LANI9
Method
Scan
TLCAIPTLC-Eualuation (CAtS Ui.M. ~:81M
Substance: 1
Di.:nsion:
track Sl
rm
cal i
area
X(calc)
1
2
3
1
2
3
4
4
5
6
7
a
9
18
11
12
13
14
15
16
17
1a
19
5
6
7
a
9
a
b
c
d
e
r
g
h
1
J
SPECT~UM
nethqd
1
End
/ Sc3 U1.13. ~:8Z31)
p.d.eu.range:
Jig
57 . 9
8 . 1 4 79.4
59.a
8.1
472.1
59 . 3
8 . 1 412. 5 .
59 . 4
8 •1
47 t. 9
59.9
8.1
471.5
59.9
8.1
469.9
59.7
8,2
472.3
59 . 4
8 .2
469 . 5
59 . 4
8 .2
4 7 t. 1
5a.a
471.4
69.2
1978. 1
69.3
1969.9
69,8
1969.a
69.8
1967.9
6a.a
1e6a.3
69.8
1869,4
69.4
1867.a
68,6
1869,5
63.4
1878.3
U4,B4 S/N:84B1ABB1
CAMAG SOFTUABE Ccl 1996
~
5
9:34
HE£P
f.t.J
YJ
SCANNER 3:
:n: tANI ,_
Uld~a
nandala
Scan Integrat Ign IMiuiillehl Spee$run
21/JUL/2888 9:4a
Data End
HlfP
YJ
(CAts Uot.M. SAI:M81M81 / Sc3 U1.13. SAI:eze381)
TLCAIPTLC-Eualuatian
Substance: 1
traclc Sl
tm
cali
1
21/JUL/2888
Data
64,7
Substance: 1
SI
tm
8.2
area
P!J
Dl-=nslon:
X(calc)
p.cleu.range:
186a.5
P .cleu.range:
area: .ean
CU (:.'.]
No result for this substance available,
n
5 :.'.
5
~
t.t.J
828391
Lampiran 8
Area LOD dan LOQ Rhodamin B
SPECTRUM
:M: LANU8
Uidya r~andl
21/JUL/2888 9:34
Method Scan Integratlgn liliddliildli Spectrun Data End
H&tP
nCAtPTLC-Eualuation (CATS U1.e1. SJ'ft:8181A881 / Sc3 U1.13, s..-tt:eze39U
Y]
Substance : 1
DI .ens ion:
pg
p.deu.range:
5 "Track Sl
I1D
cal i
area
XCcalc)
No peak detected.
1
1
2
2
No peak detected,
3
3
No peak detected,
4
4
No peak detected,
5
5
~peak
detected,
6
6
No peak detected,
7
7
·No peak detected.
8
8
No peak detected.
9
9
No peak detected,
18
a
No peak detected.
11
b
59.2
323,6
12
c
59.3
471.5
13
d
59.8
583,5
14
e
59.8
584:.4
15
f
58.8
758,6
16
g
59.8
855.9
17
h
59.4
972.8
18
68.6
1849.5
19
j
No peak detected.
t•J
Substance: 1
Sl
11D
area:
-=an
P.deu.range:
5 "CU [X]
n
CAMAG SOFTUARE Cc) 1996
88
SCANNER 3:
828381
Lampiran 9
Area Akurasi dan Presisi Rhodamin B
SPECTRUM
:M: LANlll
Uid~a
nandala
Method Scan Integration libb,)Jiiiuj.l Spectrun
22-'JUL/2eee
Data
End
9:18
HEkf
tLCAtPnc-Eualuation (CATS IH.&i, SA1:&4e1Ae81 / Sc3 U1.13, SAI:8283e1l t•Jt•l
Di..ension:
Jig
p.deu.range:
5 %
Substance: 1
X(calc)
cali
track SI
area
tm
57.e
1
1
e. 1 473.5
2
2
56.9
e .1 762.8
3
3
57.2
e .1 856.8
4
1
58.e
e .1 975.3
58,8
5
5
e .1 1EI5Z.3
6
63.0
a
1557.3
7
63.0
1514.6
b
62.7
a c
1536.4
62.7
9
d
1529.3
lEI
e
62.6
1571.8
f
62.6
11
857.8
g
12
62.4
847.3
h
86_1,7
13
62.6
14
63.1
852.4
j
15
63.4
871.9
Substance: 1
P.deu.range:
5%
area: aean
CU [%]
n
tm
SI
62.6
••••
••
e
a
b
62.6
••••
••
e
c
62.4
159,3te ng
••
1
62.6
••••
••
e
d
U4.B4 S/N:EI4B1ABB1
CAMAG SOFTUARE Ccl 1996
89
SCANNER 3:
B2e3e1
Lampiran 10
Area Kadar Sampel
SPECTRUM
22/JUL/2888 9:48
Data End
H&EP
TLCAiPTLC-Eualuation (CATS Ui.&i. SAt:&i81Mel / Sc3 U1.13. SAt:828381)
p.dcu.rangc:
Di..:nsion:
pg
Substance: 1
5%
X(calc)
nD
cali area
Traclc Sl
57,8
1
473.5
1
8.1
56.9
2·
8. 1 762.8
2
57.2
3
856.8
3
8.1
58.8
4
4
8.1
975.3
58.8
5
5
8.1 1852,3
a
63.8
958.8
6
b
995,4
7
63.8
c
62.7
933.9
8
d
62.7
1829.2
9
e
62.6
18
889.3
f
62.6
11
861.3
g
826,7
62.4
12
h
62.6
842.8
13
Method
:M: LANI12
Sc:an
Substance: 1
Sl
a
b
c
d
nandala
Uid~:a
Integrat !on lldn1ijiii.hi Spec:trurt
P .dcu .range:
5%
[%]
n
62,6
8
****
**
62.6
8
****
**
62,4
59.318 ng
1
**
62,6
8
****
**
U4.84 S/N:8481A881
CAMAG SOFTUAHE Cc) 1996
nD
area: .:an
t•J •J
cu
90
SCANNEH 3:
828381
S?!CTRUn
:n: LANI13
22/JUL/2eea 9:34
Dda End
HifP
nCAIPTLC-Eualuation (CATS Ui.EH. SA1:9191.Aee1 / Sc3 U1.13. SAt:9Z93ell t•J ,.J
p.dcu.rangc:
5%
Substdna:: 1
Di.:nsion:
Jig
X(calc)
cali
Track SI
nD
area
473,5
1
1
57.a
a. 1
2
2
a. 1
762.8
56,9
e. 1
3
57.2
856.8
3
4
a. 1
4
975.3
58.8
5
a .1 tesz.3
5
58.8
59,9
954.3
6
a
59,7
1816,4
7
b
59,4
c
8
992.2
d
59.4
9
1a 13. 1
e
58,8
te
733.7
f
11
59.2
8a3.9
g
59,3
12
729.5
h
59,8
13
7·19. a
14
59.8
874.1
j
58,9
15
998.3
k
16
59.a
884,6
59,4
17
1
992.6
Method
Scan
Substance: 1
SI
tm
Uidya "andala
Integrat jon lltl1b.Jiiii1Uli Spectrul"'
P .deu.range:
area:
-=an
CU [;d
5
:1.
n
CAMAG SOFTUAFIE
91
Cc)
't996
SCANNEFI 3:
a2a3a1
Lampiran 11
NATIONAL OUAUTY CONTROL LABORATORY OF
ORUG AND FOOD
PUSAT PEMEAIKSAAN 08AT DAN MAKANAN
Di