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. 2012 Feb 16;4(1):51–59. doi: 10.1016/j.jare.2012.01.003

Table 1.

Results of assay validation parameters obtained by applying the proposed methods.

Parameter Ezetimibe
Atorvastatin calcium
IS
D1 224.6 nm 238.6 nm TLC-densitometry D1 D2 TLC-densitometry
Concentration range 10.00–30.00 (μg mL−1) 10.00–35.00 (μg mL−1) 5.00–30.00 (μg mL−1) 0.10–0.60 (μg band−1) 10.00–35.00 (μg mL−1) 10.00–35.00 (μg mL−1) 0.10–0.60 (μg band−1)



Linearity
Slope 0.0170 0.0365 0.0430 4656.6857 0.0060 0.0349 5165.4857
Intercept 0.0219 0.0137 0.0316 −190.7733 −0.0012 −0.0047 76.7133
Correlation coefficient (r) 0.9995 0.9995 0.9997 0.9998 0.9998 0.9994 0.9999
Standard error of the slope 0.0003 0.0006 0.0005 42.5386 0.00005 0.0006 33.3275
Confidence limit of the slope 0.0170 ± 0.0008 0.0365 ± 0.0016 0.0430 ± 0.0014 4656.6857 ± 118.1060 0.0060 ± 0.0002 0.0349 ± 0.0017 5165.4857 ± 92.5321
Standard error of the intercept 0.0057 0.0140 0.0095 16.5664 0.0013 0.0144 12.9792
Confidence limit of the intercept 0.0219 ± 0.0158 0.0137 ± 0.0389 0.0316 ± 0.0265 −190.7733 ± 45.9957 −0.0012 ± 0.0036 −0.0047 ± 0.0399 76.7133 ± 36.0361
Accuracy (Mean ± S.D.) 100.23 ± 1.62 99.75 ± 1.43 99.80 ± 0.95 99.77 ± 1.30 99.58 ± 0.84 99.72 ± 1.36 99.86 ± 0.97



Precision (RSD %)
Repeatabiltya 0.96 0.45 0.48 1.00 1.24 1.14 0.97
Intermediate precisionb 1.16 1.31 1.10 1.40 1.32 1.34 1.29
Specificity 99.66 ± 1.03 100.89 ± 0.89 100.47 ± 0.81 100.25 ± 0.82 99.39 ± 0.81 100.47 ± 1.06 100.49 ± 0.78
Limit of detection (LOD)c 2.70 μg mL−1 3.10 μg mL−1 1.79 μg mL−1 0.03 μg band−1 1.75 μg mL−1 3.33 μg mL−1 0.02 μg band−1
Limit of quantitation (LOQ)c 8.19 μg mL−1 9.41 μg mL−1 5.43 μg mL−1 0.09 μg band−1 5.31 μg mL−1 10.09 μg mL−1 0.06 μg band−1

LOD = (SD of the response/slope) × 3.3; LOQ = (SD of the response/slope) × 10.

a

The intraday (n = 3), average of three concentrations repeated three times within day.

b

The interday (n = 3), average of three different concentrations repeated three times in three successive days.

c

Limits of detection and quantitation are determined via calculations.