Application of experimental design for the optimization of forced degradation and development of a validated stability-indicating LC method for luliconazole in bulk and cream formulation

Abstract

A stability-indicating LC method was developed and validated for the determination of luliconazole in bulk and cream formulation. Luliconazole was exposed to acid, alkali and water hydrolysis, oxidation effect by hydrogen peroxide, dry heat and photolytic conditions. Full factorial design was used during forced degradation experiments and the factors/combination of factors which were most likely to effect degradation of luliconazole under various conditions were identified and further were optimized using surface response curve. Drug was found to be stable under wet heat and dry heat conditions, but substantial degradation was observed under acid, alkali, oxidative and photolytic conditions. Drug and its degradation products were optimally resolved on HiQ sil C-18HS (250×4.6mm, 5μm) column with the mobile phase consisting of methanol and water (80:20, v/v) at a flow rate of 1mL/min, detection was performed at 296nm. The procedure was validated for specificity, linearity, accuracy and precision. There was no interference of excipients and degradation products in the determination of active pharmaceutical ingredient. The method was accurate and precise and the response was found to be linear in the range of 2–14μg/mL. The method was found to be simple and fast by making use of experimental design.