Development and validation of Stability Indicating RP-HPLC Method for the Determination of Axitinib in Bulk and its Pharmaceutical Formulations

[摘要] This paper presents a novel, simple, accurate and cost-effective Stability-indicating Reverse-Phase High- Performance Liquid Chromatography method for determination of Axitinib in bulk drug and forced degradation products in the pharmaceutical formulation was developed and validated. The current chromatographic separation was achieved with the Altima C18, (150 × 4.6 mm 5μm) column with a mobile phase used a mixture of acetonitrile and KH2PO4 (60:40, v/v %). The temperature of the column at 30ºC with a flow rate of 1.0 ml/min and wavelength set at 338 nm. The retention time of axitinib was 4.27 min respectively. Drug product was subjected to stress conditions of acidic, alkaline, oxidative, thermal, hydrolytic, photochemical degradation. All the degradation products were well separated from axitinib it’s highly sensitive towards acid, base and peroxide degradation. The developed method was validated statistically, parameters such as specificity, accuracy, precision, limit of detection, limit of quantification and robustness as per the ICH guidelines. The linearity dynamic range 25-250 μg/ml and effective mean percentage recoveries were 99.63% and LOQ, LOD values of axitinib were found to be 0.62 and 1.88 μg/ml, where recovery were 99.37% - 99.87 % respectively. Statistical analysis of the suggested method and reference method using student ‘t-test‘ and the F-ratio test, reveals that this suggested method demonstrated greater accuracy and sensitivity compared to the existing reference method. This method can be applied in different aspects like drug testing and routine analysis in quality control of pharmaceutical industries.

[学科分类] 药理学