1458
K
oshy
et al
.:
J
ournal of
AOAC I
nternational
V
ol
.
99, N
o
.
6, 2016
response factors, providing data on finished products, clarifying
the discard volume in the filtration step, and determining the
LOQ of the method.
References
(1) Mirjalili, M.H., Moyano, E., Bonfill, M., Cusido, R.M., &
Palazón, J. (2009)
Molecules
14
, 2373–2393. doi:10.3390/
molecules14072373
(2) Ichikawa, H., Takada, Y., Shishodia, S., Jayaprakasam, B.,
Nair, M.G., & Aggarwal, B.B. (2006)
Mol. Cancer
Ther.
5
, 1434–1445. doi:10.1158/1535-7163.
MCT-06-0096
(3)
Official Methods of Analysis
(2015) AOAC
INTERNATIONAL, Rockville, MD,
SMPR 2015.007
(4)
Official Methods of Analysis
(2012) AOAC
INTERNATIONAL, Rockville, MD,
Appendix K
Table 13. Analysis of withanolide content under intermediate precision conditions
Sample No.
Condition
Content, % w/w
Mean of sum,
% w/w RSD of sum, %
W-IV W-V WF-A
12-D
W-A
W-B Sum
WS/06Lot08
1
0.917 0.650 0.659
0.284
0.225
0.066 2.802
2.888
4.21
2
1.071 0.629 0.608
0.304
0.290
0.071 2.974
WS/06Lot10
1
0.911 0.621 0.616
0.267
0.205
0.062 2.681
2.749
3.50
2
1.047 0.601 0.561
0.282
0.258
0.067 2.817
WS/05Lot20
1
0.067 0.044 0.081
0.022
0.021
0.005 0.241
0.252
6.17
2
0.080 0.044 0.083
0.024
0.027
0.001 0.263
WS/05Lot21
1
0.478 0.310 0.410
0.125
0.102
0.029 1.453
1.495
3.97
2
0.538 0.298 0.415
0.130
0.128
0.027 1.537
RD/1170
1
0.848 0.594 0.700
0.332
0.229
0.076 2.779
2.900
5.88
2
0.995 0.599 0.740
0.257
0.348
0.080 3.020
RD/1045
1
0.606 0.364 0.402
0.248
0.131
0.042 1.793
1.850
4.32
2
0.744 0.357 0.422
0.140
0.201
0.043 1.906
RD/1162
1
0.152 0.090 0.100
0.021
0.025
0.004 0.391
0.389
0.91
2
0.162 0.083 0.090
0.022
0.025
0.000 0.386
ERH-46
1
0.184 0.148 0.145
0.041
0.041
0.010 0.570
0.586
3.74
2
0.213 0.147 0.141
0.046
0.043
0.011 0.601
Table 14. Stability of withanolide content in the sample solution over 24 h at room temperature
Time
Withanolide content, % w/w
W-IV
W-V
WF-A
12-D
W-A
W-B
Sum
0 h
0.399
0.319
0.413
0.123
0.107
0.030
1.390
24 h
0.409
0.350
0.415
0.122
0.110
0.030
1.435
Difference
0.010
0.031
0.002
−0.001
0.003
0.000
0.045
% Difference from
t
=0
2.51
9.72
0.48
−0.81
2.80
0.00
3.24
63