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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