Development and validation of ultra-performance liquid chromatography method for the determination of meloxicam and its impurities in active pharmaceutical ingredients

Abstract

The main objective was to develop a suitable and rapid ultra-performance liquid chromatography (UPLC) method for the quantitative determination of meloxicam and its impurities. Starting from data in literature, we calculated the new parameters to translate a high performance liquid chromatography method used for the analysis of meloxicam with its major degradation products to UPLC method, and then we switched on many trials to optimize and improve its analytical performance. Chromatographic separation was achieved on ACQUITY UPLC HSS-T3 (2.1×100mm, 1.8μm). The eluted compounds were monitored at 260nm and 350nm. The flow rate was set at 0.4mL/min, injection volume at 0.8μl, and the column oven temperature was maintained at 45°C. The developed method was validated according to the International Conference on Harmonisation (ICH) guidelines for specificity, linearity, accuracy, precision, robustness, quantification limit, detection limit; and then applied to stability study of meloxicam subjected to different ICH prescribed stress conditions (hydrolysis, oxidation, heat and photolysis). The results show that the new UPLC method enables separation of meloxicam from its impurities in only 5min with a total mobile phase consumption of 1.8mL. All impurities get separated with good peak shapes and resolution factor greater than 2. The new method indicates stability and proved to be specific, precise accurate with linear correlation between concentrations and peak areas, allowing gain of more than six times analysis and more than twenty times solvent consumption, so in cost. Therefore, it can be beneficial for pharmaceutical industrial output.