Table 4 Method validation data.

From: AQbD based green UPLC method to determine mycophenolate mofetil impurities and Identification of degradation products by QToF LCMS

Test

Details

Acceptance Criteria

Results

Imp-E

Imp-A

Imp-H

Imp-D

MPM

Imp-F

Imp-B

Imp-C

Imp-G

Specificity

Retention time

n = 1, each impurity at 1.0 µg mL−1

Each peak should elute at a different retention time

4.953

5.418

6.137

6.509

6.871

7.146

7.289

7.658

9.820

There are no peak interferes with placebo peaks. All the individual impurity peaks eluted at different retention times

Linearity

Range (µg mL−1)

Range (µg mL−1)

0.0371–0.7545

0.0321–0.7321

0.0233–0.7508

0.0467–0.7509

0.0333–0.7497

0.0293–0.7678

0.0363–0.7584

0.0347–4.9634

0.0436–0.7636

Minimum 6 concentration levels in the range LOQ–150% of specification

Correlation coefficient should be > 0.999

0.999

0.999

0.999

0.999

0.999

0.999

0.999

0.999

0.999

Slope

 

44,357.242

60,717.374

138,890.406

66,685.223

71,979.649

86,647.962

90,671.303

101,629.307

83,134.619

Intercept

 

1759.467

58.533

− 237.267

− 501.467

1041.667

− 82.800

− 121.667

− 770.800

− 475.467

STEYX SD

 

520.919

121.679

264.279

515.648

71.593

229.146

390.461

719.195

283.291

Limit of detection

0.01 µg mL−1 (lowest detectable concentration)

S/N ratio > 3

0.011

0.010

0.007

0.014

0.010

0.009

0.011

0.010

0.013

Limit of quantitation

0.03 µg mL−1 (lowest quantitatable concentration)

S/N ratio > 10

0.037

0.032

0.023

0.046

0.033

0.029

0.035

0.034

0.043

Accuracy

n = 9 (3 determinations each at LOQ, 50%, 100% and 150% specification level

Recovery at each level should be 90–110%

99.8 ± 1.1

100.2 ± 3.0

98.0 ± 2.1

99.7 ± 3.0

100.6 ± 2.6

101.0 ± 3.2

98.2 ± 0.8

102.4 ± 2.1

102.1 ± 2.9

100.5 ± 3.8

99.7 ± 2.0

100.7 ± 2.4

98.5 ± 2.5

98.2 ± 3.1

98.0 ± 2.2

98.1 ± 1.2

102.7 ± 2.0

100.1 ± 2.9

99.9 ± 0.5

100.5 ± 3.3

96.2 ± 1.9

96.7 ± 1.0

99.3 ± 0.5

98.2 ± 1.9

99.8 ± 2.3

100.3 ± 2.9

98.3 ± 2.3

101.5 ± 2.6

98.9 ± 3.8

100.6 ± 2.1

97.8 ± 1.2

100.0 ± 2.9

98.4 ± 1.3

101.4 ± 1.7

101.3 ± 2.5

99.5 ± 1.7

Precision (Analyst 1)

n = 6 (6 determinations each at 1.0 µg mL−1)

RSD should be < 5%

1.6%

2.5%

2.8%

2.8%

2.2%

1.6%

3.0%

1.5%

2.1%

Intermediate precision (Analyst 2)

n = 6 (6 determinations at µg mL−1)

RSD should be < 5%

4.5%

0.8%

1.6%

2.1%

3.3%

1.9%

1.2%

1.8%

2.2%

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