Development and Validation of Stability Indicating UFLC Method for the Estimation of Anti-spasmodic Drug - Valethamate Bromide

Abstract

A stability indicating Ultra-Fast Liquid Chromatography (UFLC) method has been developed to estimate valethamate bromide (V&B) in tablet dosage forms and to separate analyte from other degradants and to carryout forced degradation studies. The chromatographic separation was achieved by using phenomenex kinetex 5 μ C18 100A (250x 4.6 mm) column with a flow rate of 1 mL/min in an isocratic mode with the mobile phase consisting of 0.05 M potassium dihydrogen phosphate buffer pH 7.5 (adjusted with potassium hydroxide) and acetonitrile in the ratio of 50:50. The eluents were monitored with PDA detector at 227 nm. In this developed method valethamate bromide was eluted at a retention time of 4.4 ± 0.1 min. The proposed method is having linearity in the concentration range of 2-12 μg/mL. The present method was successfully validated with respect to system suitability, linearity, precision, accuracy, limit of detection (LOD), limit of quantification (LOQ) and robustness as per international council for harmonization (ICH) guidelines. The drug was subjected to different degradation conditions like acid and alkali hydrolysis, oxidation, thermal and UV radiation etc. Peak purity of the drug was passed in all degradation conditions which demonstrated the specificity of assay method for it in presence of degradation products. The proposed method can be applied for determination of valethamate bromide in pure drug and in pharmaceutical formulation.