1.

kurva kalibrasi

standar kadar (%) area

std 1 0 0.108
std 2 0.1 0.728
std 3 0.5 5.165
std 4 1 9.26
std 5 2 16.399
std 6 4 31.707
std 7 5 47.108
slope 8.830632
intercept -0.112995
correlation coefficient ® 0.993513

2. pengukuran karutan standar tengah (Laboratory control standar/LCS)

standar kadar (%) area CLCS %R LLCS

std 1 9.26 1.061418 106.1418

3. penentuan trueness, bias, dan presisi metode

ulangan area C (%) %T % bias

1 2.049 0.244829 97.93159 -990207
2 2.174 0.258984 103.5937 -989641
3 2.184 0.260117 104.0467 -989595
4 2.169 0.258418 103.3672 -989663
5 1.544 0.187642 75.05667 -992494
6 2.157 0.257059 102.8237 -989718
7 2.043 0.24415 97.65981 -990234
8 1.952 0.233844 93.53779 -990646
9 2.198 0.261702 104.6808 -989532
10 2.785 0.328175 131.2701 -986873
rearata 0.253492 101.3968 -989860
simpangan baku 0.034385
%RSD 0.135643

4. penentuan MDI dan LoQ

Ulangan area C(%) %R

1 0.817 0.105315 10.53146
2 0.862 0.110411 5.520525
3 0.761 0.098973 3.299102
4 0.756 0.098407 2.460171
5 0.833 0.107126 2.14253
6 0.783 0.101464 1.691073
7 0.861 0.110297 1.575675
8 0.829 0.106674 1.333419
 9 0.797 0.10305 1.144997
10 0.705 0.092631 0.926315
rerata 0.103435
simpangan baku 0.00567
%RSD 5.481671
S/N 1824.261
MDL 0.017821
LoQ 0.0567
MDL estimasi 0.02268

5. Penentuan LOL (Level of linearity)

C Area 1 Area 2 Area 3 Area 4 Area 5 Area 6 Area 7 Area 8

0,1 % 0.817 0.862 0.761 0.756 0.833 0.783 0.861 0.829

5% 39.966 47.108 42.466 40.378 39.122 45.031 47.15 40.275

6. Repeatabolitas, reprodusibilitas, dan efek matriks

a. penentuan reprodusibilitas pada konsentrasi 0,1%
ulangan area C% %RPD %R % bias
1 2 rerata
1 0.817 0.783 0.8 0.103389 4.25 103.3895 3.389492
2 0.862 0.861 0.8615 0.110354 0.116077 110.3539 10.35389
3 0.761 0.829 0.795 0.102823 -8.553459 102.8233 2.823281
4 0.756 0.797 0.7765 0.100728 -5.280103 100.7283 0.728301
5 0.833 0.705 0.769 0.099879 16.64499 99.87898 -0.121015
rerata 0.103435 1.435502 103.4348 3.434789
simpangan baku 0.00413
%RSD 3.992594
Nilai horwitz 2.814087

b. pennetuan reprodusibiltas pada konsentrasi 5%

ulangan area C% %RPD %R % bias
1 2 rerata
1 39.966 45.031 42.4985 4.825419 -11.91807 96.50837 -3.49163
2 47.108 47.15 47.129 5.349786 -0.089117 106.9957 6.995728
3 42.446 40.275 41.3605 4.696549 5.248969 93.93098 -6.069022
4 40.378 42.775 41.5765 4.721009 -5.765276 94.42018 -5.579816
5 39.122 42.775 40.9485 4.649893 -8.920962 92.99786 -7.002137
rerata 4.848531 -4.288891 96.97062 -3.029375
simpangan baku 0.287493
%RSD 5.929483
Nilai horwitz 1.577013

Efek Matriks
Komponen Area C% y z v g
I II rerata
CU 2.122 1.953 2.0375 0.243527

CU+spike 34.673 39.59 37.1315 4.217648 0.1 100 10 1

7. bagian kendali
a. akurasi
data %R rata-rata rata" - 2sd rata" + 2sdrata" - 3sd rata" + 3sd
1 103.3895 100.2027 88.56129 111.8441 82.74059 117.6648 120

2 110.3539 100.2027 88.56129 111.8441 82.74059 117.6648 115

3 102.8233 100.2027 88.56129 111.8441 82.74059 117.6648 110
4 100.7283 100.2027 88.56129 111.8441 82.74059 117.6648 105
5 99.87898 100.2027 88.56129 111.8441 82.74059 117.6648 100
6 96.50837 100.2027 88.56129 111.8441 82.74059 117.6648 95
7 106.9957 100.2027 88.56129 111.8441 82.74059 117.6648 90
8 93.93098 100.2027 88.56129 111.8441 82.74059 117.6648 85
9 94.42018 100.2027 88.56129 111.8441 82.74059 117.6648 80
10 92.99786 100.2027 88.56129 111.8441 82.74059 117.6648 75
rerata 100.2027 0 2
sd 5.820707

b. presisi
data %RPD rata-rata rata" - 2sd rata" + 2sdrata" - 3sd rata" + 3sd
1 4.25 -1.426695 -18.53082 15.67743 -27.08289 24.2295
2 0.116077 -1.426695 -18.53082 15.67743 -27.08289 24.2295 30
3 -8.553459 -1.426695 -18.53082 15.67743 -27.08289 24.2295
4 -5.280103 -1.426695 -18.53082 15.67743 -27.08289 24.2295 20
5 16.64499 -1.426695 -18.53082 15.67743 -27.08289 24.2295
10
6 -11.91807 -1.426695 -18.53082 15.67743 -27.08289 24.2295
7 -0.089117 -1.426695 -18.53082 15.67743 -27.08289 24.2295 0
0 2
8 5.248969 -1.426695 -18.53082 15.67743 -27.08289 24.2295
9 -5.765276 -1.426695 -18.53082 15.67743 -27.08289 24.2295 -10
10 -8.920962 -1.426695 -18.53082 15.67743 -27.08289 24.2295
-20
rerata -1.426695
sd 8.552065 -30
Area 9 Area 10 Sd
0.797 0.705 0.0500692853

42.775 45.399 3.0340249395

 %Recovery

397.4121

Chart Title
120
115
110
105
100
95
90
85
80
75
0 2 4 6 8 10 12

rata-rata rata" - 2sd rata" + 2sd

rata" - 3sd rata" + 3sd Column B

Chart Title
30

20

10

0
0 2 4 6 8 10 12
-10

-20

-30

%RPD rata-rata rata" - 2sd

rata" + 2sd rata" - 3sd rata" + 3sd
 LAMPIRAN
RINGKASAN HASIL VERIFIKASI METODE PENGUJI

Acuan metode penguji :

Parameter :
Bidang pengujian :
Rentang pengujian :
Nama personil :
Tanggal pengujian :

Uraian Hasil
Trueness %R = 101.3968

Bias metode % Bias = -989860

% RSD = 0.135643
Presisi metode
%CVHorwitz =
%R =
%RSD = 5.481671
Batas deteksi
S/N = 1824.261
dengan metode
(MDL) MDL = 0.017821
Spike = 1

Batas linearitasi
LoQ = 0.0567
LoQ

r=
a≤ MDL
Batas linearitas P atau significance f=
value
(LoL)
Fhitung =
Ftabel =
% RSDkadar rendah =
Reprodusibilitas % RSDkadar tinggi =
0,67%CVHorwitz =
Reprodusibilitas % RSDR =
Efek matriks %R = 397.4121
Bagan kendali Plotkan dalam bagan kendali

o   Metode terverifikasi

sesuai persyaratan teknis
Kesimpulan
o   Tidak terpenuhi
o   Metode terverifikasi
sesuai persyaratan teknis
o   Tidak terpenuhi

Catatan : peraturan mengacu pada :

%RSD ≤ %CVHorwitz jika pengujian tidak mencantumkan batas keberterimaan
Disiapkan oleh Data diverifikasi oleh
 LAMPIRAN
RINGKASAN HASIL VERIFIKASI METODE PENGUJIAN

Batas Keberterimaan
%R = 85 -115%

Jika batas kebeterimaan trueness diterima. Maka bias

metode diterima

%RSD ≤ %CVHorwitz =

%R = 85 -115%
%RSD ≤ %CVHorwitz =
S/N = 2,5 – 1,0
MDL < kadar spike
Kadar spike < 10 MDL

Jika MDL diterima, maka LoQ diterima

Uji linearitas :
Koefisien (r) ≥ 0,995
%RLCS = 100% ± 10%
Pvalue atau significance f ≤ 0,05
Uji F :
Fhitung < Ftabel

%RSD ≤ 0,67%CVHorwitz

%RSD ≤ 0,67%CVHorwitz
%R = 90 – 110%
 Tidak ada kecenderungan dan masuk batas
keberterimaan

a pengujian tidak mencantumkan batas keberterimaan

Data divalidasi oleh
ODE PENGUJIAN

Keterangan