Forced degradation study to develop and validate stability-indicating RP-LC method for the determination of ciclesonide in bulk drug and metered dose inhalers

摘要

A simple, selective and precise stability-indicating reversed-phase liquid chromatographic method was developed and validated for the determination of ciclesonide. Ciclesonide was subjected to acid and alkali hydrolysis, oxidation, thermal and photo-degradation. The degradation products were well separated from the pure drug. The method was based on isocratic elution of ciclesonide and its degradation products on reversed phase C18 column (250 mm × 4.6 mm, 10 μm) - Phenomenex using a mobile phase consisting of ethanol-water (70:30, v/v) at a flow rate of 1 mL min~(-1). Quantitation was achieved with UV detection at 242 nm. Linearity, accuracy and precision were found to be acceptable over the concentration range of 5-200 μg mL~(-1). Desisobutyryl-ciclesonide was prepared by selective alkaline hydrolysis of the ester and proved to be the main degradation product. The proposed method was successfully applied to the determination of ciclesonide in bulk and in its pharmaceutical preparation.