The described method is linear in the range of 01 \u03bcg mL 1to 2 \u03bcg mL 1 of each

The described method is linear in the range of 01 μg

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and purity data is listed in table II. The described method is linear in the range of 0.1 μg mL -1 to 2 μg mL -1 of each impurity, demonstrated acceptability of the method for the quantitative determination in that range. The rela- tive response factor (RRF) of Impurity-A, Impurity-B, Impurity-C with respect to PNT was found to be 1.13, 0.93 and 0.59 respectively. The value of linearity range, equation, corellation coefficient, LOD and LOQ for PNT and its related impurity are shown in Table III. In the precision study, the percentage relative stan- dard deviation (RSD) of six replicates was found less than 0.13 % for retention time and 1.12 % for peak area of all the impurities and PNT, indicating good repeatability of the method. The results of the reproducibility study under a different set of conditions are also in the same order of magnitude. The percentage bias between two different sets of conditions for retention time and peak area was within ±1.29 and ±0.29 respectively for all the impurities and PNT, indicates that method is rugged for its intended use. The method showed excellent recovery (accuracy) at three different studied concentrations QL, 100 and 200 % of specification level for all the impurities. The mean re - coveries of all the impurities and PNT were found to be in the acceptable range of 97.94 to 102.6 %. Table IV shows all the data related to accuracy and precision. FIGURE 2- Typical chromatogram for A) PNT with impurities; B) Under acidic condition and C) Under oxidative condition. TABLE II - Results of specificity and purity data Name Relative Retention time Peak purity Purity threshold Pantoprazole 1.00 0.957 4.685 Impurity-A 0.80 3.984 7.596 Impurity-B 1.66 9.961 18.879 Impurity-C 0.57 2.331 4.355 TABLE III - Linearity, LOD and LOQ results for PNT and related impurities Compound Linearity LOD & LOQ (µg mL -1 ) Equation Range (µg mL -1 ) Correlation coefficient Response Factor PNT Y=46517x-496 0.13-2 0.9994 1 0.043& 0.129 Impurity A Y=41112x+422 0.14-2 0.9997 1.13 0.046 &0.138 Impurity B Y=49906x+328 0.14-2 0.9991 0.93 0.047&0.140 Impurity C Y=78900x-1399 0.13-2 0.9996 0.59 0.045&0.134
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A validated stability indicating HPLC method for the determination of process-related impurities in pantoprazole bulk drug and formulations 181 TABLE V - Robustness data Robustness Parameter Relative retention Time Resolution % RSD (n=6) Impurity-A Impurity-B Impurity-C Control 0.80 1.66 0.57 4.92 2.30 Flow rate (–10%) 0.80 1.60 0.59 4.25 0.23 Flow rate (+10%) 0.79 1.65 0.56 4.36 1.21 Column Oven Temp. (-5 °C) 0.80 1.64 0.61 4.94 0.82 Column Oven Temp. (+5 °C) 0.75 1.64 0.57 4.96 1.22 pH Change (– 0.2 pH units) 0.84 1.59 0.59 4.72 2.89 pH Change (+ 0.2 pH units) 0.68 1.76 0.62 4.84 1.99 Gradient change (–2 % absolute) 0.86 1.55 0.55 4.73 1.58 Gradient change (+2 % absolute) 0.83 1.69 0.56 3.30 1.85 Wavelength (–5 nm) 0.86 1.60 0.56 5.21 0.15 Wavelength (+5 nm) 0.86 1.60 0.56 5.24 0.35 TABLE VI - Assay of pantoprazole and its main impurities in pharmaceuticals Formulation Amount, %±SD PNT Impurity-A Impurity-B Impurity-C Pantosec 40 (tablet) 99.04±0.98 0.094±0.58 0.021±0.93 0.11±0.83 Allpan 40 (tablet) 101.23±1.81 0.075±0.61 0.072±1.09 0.089±0.41 Altopan- i.v. (injection) 98.34±2.30 0.092±0.33 0.088±0.34 0.061±1.02 TABLE IV - Precision and Accuracy data Compound ART (Min) % RSD (n=6) % Bias APA % RSD (n=6) % Bias Average Accuracy±SD % RSD OC DC OC DC PNT 8.11 8.12 0.11 0.12 18480516.73 18480519.12 1.09 0.00 102.6±0.81 0.81 Impurity-A 6.63 6.61 0.13 0.30 57466 57482.42 0.89 0.03 101.64±2.3 1.10 Impurity-B 13.15 13.32 0.7 1.29 25339.79 25414.21 0.91 0.29 103±1.93 1.88 Impurity-C 4.62 4.58 0.09 0.87 36404.28 36492.18 1.12 0.24 97.94±1.91 1.96
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