Determination of lumiracoxib by a validated stability-indicating MEKC method and identification of its degradation products by LC-ESI-MS studies

Abstract

A stability-indicating MEKC method was developed and validated for the analysis of lumiracoxib (LMC) in pharmaceutical formulations using nimesulide as the internal standard (IS). Optimal conditions for the separation of LMC and degradation products were investigated. The method employed 50 mM borate buffer and 50 mM anionic detergent SDS solution at pH 9.0. MEKC method was performed on a fused-silica capillary (50 μm id; effective length, 40 cm) maintained at 30°C. The applied voltage was 20 kV and photodiode array (PDA) detector was set at 208 nm. The method was validated in accordance with the International Conference on Harmonisation requirements. The stability-indicating capability of the method was established by enforced degradation studies combined with peak purity assessment using PDA detection. The degradation products formed under stressed conditions were investigated by LC-ESI-MS and the two degraded products were identified. MEKC method was linear over the concentration range of 5-150 μg/mL (r(2) =0.9999) of LMC. The method was precise, accurate, with LOD and LOQ of 1.34 and 4.48 μg/mL, respectively. The robustness was proved by a fractional factorial design evaluation. The proposed MEKC method was successfully applied for the quantitative analysis of LMC in tablets to support the quality control.