Development and validation of analytical methods and impurity profiling for some antihypertensive drugs in dosage forms

Abstract

The present work represents specific, stability indicating, accurate and precise method for impurity profiling by RP-HPLC method and Elemental Impurities in anti-hypertensive drugs dosage forms. Identify and characterized the degradation impurities with different techniques like IR, Mass spectroscopy and 1H NMR Spectroscopy obtained by RP-HPLC method. The determination of Organic impurities stability indicating method is developed by RP-HPLC for Phenoxybenzamine Hydrochloride dosage form. Identify and characterized the degradation impurities i.e. 2-[benzyl(1-phenoxypropan-2-yl)amino]ethan-1-ol-Hydrochloride and 1-benzyl-1-(1-methyl-2-phenoxy-2-ethyl)-aziridiniumperchlorate which is present in Phenoxybenzamine Hydrochloride dosage form. Class I and II A Elemental impurities is determined and quantified by ICP-MS method as per ICH Q3 (D) guideline and USP chapter lt233gt for Phenoxybenzamine Hydrochloride dosage form. Specification limit of each elemental impurities (Vanadium, Cobalt, Nickel, Arsenic, Cadmium, Mercury and Lead) is selected based on the Permitted daily exposure of finished product dosage form label claim i.e. 10 mg. The degradation study was carried out under different environments like acidic, alkaline, neutral, oxidative, photolytic, humidity and thermal conditions. The developed organic impurities method was validated in terms of specificity, linearity, range, accuracy, precision, robustness, limit of detection, limit of quantitation, repeatability and system suitability as per ICH Q2 (R1) guideline. The developed elemental impurities method was validated in terms of specificity, linearity, range, accuracy, precision, limit of detection, limit of quantitation, repeatability and system suitability as per ICH Q2 (R1) guideline and USP chapter lt233gt. newlineThe calibration curve of all the developed methods were found linear over the proposed concentration range. Percentage impurity profiling and Percent recoveries of same were obtained within the limit specified as per ICH guidelin