DEVELOPMENT & VALIDATION OF STABILITY INDICATING HPLC METHOD FOR ESTIMATION OF POLMACOXIB IN SOLID DOSAGE FORM AND APPLICATION TO DEGRADATION STUDY

Abstract

Stability indicating assay method is reported for determination of polmacoxib from its capsule formulation. The polmacoxib is relatively a new molecule and very few analytical methods have been reported for its determination from biological fluid. Hence, a new simple, accurate, rapid and selective high-performance liquid chromatographic method has been developed and validated. The method was applied for stress degradation study of the drug. The separation of analyte and degradation products were obtained on Inertsil ODS 3V (250mm × 4.6mm), 5μm column, using the gradient elution of ammonium acetate buffer (Mobile Phase - A) and acetonitrile (Mobile Phase - B), with a flow rate of 1.5 mL/min. The eluent was monitored at 240 nm and the total run time was 28 min. Retention time of polmacoxib was found to be 10.8 min. Force degradation of polmacoxib was carried out under acidic, basic, oxidative, thermal, photo and humidity conditions. Polmacoxib has been found to degrade in selected oxidative degradation conditions. The developed method was validated for various parameters like system suitability, specificity, linearity, accuracy, precision, robustness, ruggedness as per ICH guidelines. The linear regression analysis data for the calibration plots showed a very good linear relationship within concentration range of 50 – 150 μg/mL with the linearity equation  Y = 19.658x + 3.434 (r² = 0.999). The method was identified as sufficiently specific to separate degradation products from the main analyte. The method had proven its potential for its application in routine estimation and stability study of polmacoxib.