Reverse Phase Liquid Chromatographic Method for Analysis of Doxofylline in Presence of its Degradation Products

Abstract

A simple, precise and novel reverse phase liquid chromatographic method for analysis of doxofylline in bulk drug as well as in pharmaceutical preparations in the presence of potential degradation products of doxofylline has been developed and validated. Forced degradation studies were carried on doxofylline in acidic, neutral and alkaline hydrolytic conditions in addition to oxidative, thermal and photolytic conditions. Optimum separation among doxofylline and its degradation products was achieved using a ternary mixture of water: methanol: ethyl acetate in the ratio of 80:10: 10 % v/v/v as the mobile phase at a flow rate of 1.0 ml/min on a Supelco C18 DB 150 mm X 4.6 mm column as the stationary phase when scanned at a wavelength of 277 nm. The retention time for the various degradation products were found to be sufficiently different with each other as well as with the parent drug at the optimized chromatographic conditions to permit their accurate quantitative estimation. The method was found to be linear at least in the range of 5- 25 μg/ml. The developed method was then validated for precision, accuracy, specificity, robustness and ruggedness in accordance with the ICH guidelines and other available regulatory guidelines.