<p><strong>Objective</strong>:<strong> </strong>To develop a rapid, accurate, linear, sensitive and stability indicating RP-HPLC method for the determination of nilotinib in bulk and pharmaceutical dosage forms in the presence of its four related substances.</p><p><strong>Methods</strong>:<strong> </strong>The RP-HPLC method was developed for the chromatographic separation of nilotinib and its impurities by using waters Xterra RP-18 (150*4.6 mm, 3.5 µm) column with a mobile phase combination of 10 mM ammonium formate with pH-3.5 and acetonitrile in gradient mode. An injection volume of 20 µl. Flow rate was 1.0 ml/min and detection was carried a wavelength of 250 nm. The method was validated as per ICH guidelines.</p><p><strong>Results</strong>:<strong> </strong>The retention time for nilotinib and its four impurities were found to be 4.37, 7.40, 8.96, 10.21 and 10.87 min respectively. The linear regression analysis data for the calibration plots showed the good linear relationship in the concentration range of 0.04-3.0 ppm for the nilotinib impurities. The % recovery of nilotinib impurities was found to be 96.8-99.4% in the linearity range. The detection limit (LOD) values were about 0.014, 0.016, 0.005 and 0.03 ppm respectively and the quantification limit (LOQ) values were 0.042, 0.048, 0.014 and 0.09 ppm respectively. The % degradation at various stress conditions like acid, alkaline, oxidative, thermal and photolytic stress was found to be 8.92, 18.35,5.63, 0.88 and 3.89 respectively.</p><p><strong>Conclusion: </strong>The RP-HPLC method compatible with LC-MS was developed for the analysis of nilotinib and its four impurities. It was validated as per the ICH guidelines and found to be linear, robust, precise, accurate, sensitive, stability indicating and can be used for routine as well as stability analysis of capsule dosage forms as well as for drug substance.</p>
A simple, rapid, sensitive and stability indicating UPLC method has been developed for the quantitative estimation of temozolomide and its impurities in bulk and pharmaceutical dosage. The separation of temozolomide and its impurities was achieved by using Acquity UPLC BEH C18-50 × 2.1 mm, 1.7 µm column maintained at 30 °C with mobile phase consisting of 0.1 % formic acid in water, pH adjusted to 2.8 and acetonitrile in a gradient programme with 12 min run time. The mobile phase flow rate was 0.4 mL/min and the UV detection was carried out at a wavelength of 270 nm. The developed method was able to separate all the process related impurities and degradants of temozolomide with proper separation and also the proposed method was mass compatible. The stability indicating power of the method was verified by performing the forced degradation studies on temozolomide using 0.1 N HCl, 0.1 N NaOH, 3 % hydrogen peroxide, photolytic and thermal degradation studies. The proposed method was validated for specificity, linearity, accuracy, precision, robustness and ruggedness parameters in accordance with ICH guidelines. The validated method can be used for the routine as well as stability analysis in the quality control laboratories.
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