New analytical methods development and identification and characterization of impurities in pharmaceuticals

Abstract

An accurate and precise gradient stability indicating reverse phase high performance liquid chromatographic method is developed for simultaneous determination of sibutramine hydrochloride and Orlistat in the newly developed capsule formulation. The chromatography equipped with Zorbax SB Phenyl (250×4.6mm) 5µ column using a mobile phase of buffer (Dissolved 7.0 g of sodium perchlorate in 1000ml water, pH adjusted to 2.1 (+ 0.05) with ortho phosphoric acid, filtered through 0.45 µ filter.) and acetonitrile, the gradient program configured with a flow rate of 2.0 ml/min, ultraviolet detector at 210nm. The retention times of sibutramine hydrochloride and Orlistat were 8 and 31 min respectively. The method linearity was studied over the range of 50 to 150 ppm with r2 of 0.9999 for sibutramine hydrochloride and 600 to 1800 ppm with r2 of 0.9999 for Orlistat. Mean recovery for sibutramine hydrochloride and Orlistat were 100.09 and 100.02 respectively A simple fast, accurate, precise, and cost effective isocratic stability indicating reverse phase high performance liquid chromatographic method is developed for simultaneous determination of Halobetasol propionate and fusidic acid as well as its impurities in the newly developed cream formulation. The chromatography equipped with Zorbax SB phenyl (250X4.6mm) column using a mobile phase of buffer (0.1% triethylamine buffer pH adjusted to 2.0 with Orthophosphoric acid) acetonitrile, methanol in the ratio of 40:35:25 v/v with a flow rate of 1.5 ml/min, with ultraviolet detector configured at 240nm. Identified all impurities and Characterization of Sibutramine Hydrochloride Impurities.