AOACSPDSMethods-2017Awardsv2

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1458 K oshy et al .: J ournal of AOAC I nternational V ol . 99, N o . 6, 2016

Table 13. Analysis of withanolide content under intermediate precision conditions

Content, % w/w

Mean of sum,

Sample No. WS/06Lot08

Condition

W-IV W-V WF-A 0.917 0.650 0.659 1.071 0.629 0.608 0.911 0.621 0.616 1.047 0.601 0.561 0.067 0.044 0.081 0.080 0.044 0.083 0.478 0.310 0.410 0.538 0.298 0.415 0.848 0.594 0.700 0.995 0.599 0.740 0.606 0.364 0.402 0.744 0.357 0.422 0.152 0.090 0.100 0.162 0.083 0.090 0.184 0.148 0.145 0.213 0.147 0.141

12-D

W-A

W-B Sum 0.066 2.802 0.071 2.974 0.062 2.681 0.067 2.817 0.005 0.241 0.001 0.263 0.029 1.453 0.027 1.537 0.076 2.779 0.080 3.020 0.042 1.793 0.043 1.906 0.004 0.391 0.000 0.386 0.010 0.570 0.011 0.601

% w/w RSD of sum, %

1 2 1 2 1 2 1 2 1 2 1 2 1 2 1 2

0.284 0.304 0.267 0.282 0.022 0.024 0.125 0.130 0.332 0.257 0.248 0.140 0.021 0.022 0.041 0.046

0.225 0.290 0.205 0.258 0.021 0.027 0.102 0.128 0.229 0.348 0.131 0.201 0.025 0.025 0.041 0.043

2.888

4.21

WS/06Lot10

2.749

3.50

WS/05Lot20

0.252

6.17

WS/05Lot21

1.495

3.97

RD/1170

2.900

5.88

RD/1045

1.850

4.32

0.389

0.91

RD/1162

ERH-46

0.586

3.74

Table 14. Stability of withanolide content in the sample solution over 24 h at room temperature

Withanolide content, % w/w

Time

W-IV

W-V

WF-A 0.413 0.415 0.002

12-D

W-A

W-B

Sum

0 h

0.399 0.409 0.010

0.319 0.350 0.031

0.123 0.122

0.107 0.110 0.003

0.030 0.030 0.000

1.390 1.435 0.045

24 h

Difference

−0.001

% Difference from t =0

2.51

9.72

0.48

−0.81

2.80

0.00

3.24

response factors, providing data on finished products, clarifying the discard volume in the filtration step, and determining the LOQ of the method.

(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

References

(1) Mirjalili, M.H., Moyano, E., Bonfill, M., Cusido, R.M., & Palazón, J. (2009) Molecules 14 , 2373–2393. doi:10.3390/ molecules14072373