Louati K, Bargaoui I, Safta F
Scientific research department, Malâa Center, road of Ain, Km 6.5, 3042 Sfax, Tunisia.
Department of analytical chemistry, University of pharmacy, road Avicenne, 5000 Monastir, Tunisia.
Ann Pharm Fr. 2018 May;76(3):187-200. doi: 10.1016/j.pharma.2018.02.001. Epub 2018 Mar 12.
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.
主要目的是开发一种合适且快速的超高效液相色谱（UPLC）方法，用于定量测定美洛昔康及其杂质。从文献数据出发，我们计算了新参数，将用于分析美洛昔康及其主要降解产物的高效液相色谱方法转换为UPLC方法，然后进行了多次试验以优化和提高其分析性能。在ACQUITY UPLC HSS-T3（2.1×100mm，1.8μm）上实现了色谱分离。在260nm和350nm波长下监测洗脱的化合物。流速设定为0.4mL/min，进样体积为0.8μl，柱温箱温度保持在45°C。根据国际协调会议（ICH）指南对所开发的方法进行了专属性、线性、准确性、精密度、稳健性、定量限、检测限的验证；然后将其应用于美洛昔康在不同ICH规定的加速条件（水解、氧化、加热和光解）下的稳定性研究。结果表明，新的UPLC方法仅需5分钟就能将美洛昔康与其杂质分离，流动相总消耗量为1.8mL。所有杂质均能得到良好的峰形分离，分离度因子大于2。新方法显示出稳定性，并被证明具有专属性、精确性和准确性，浓度与峰面积之间具有线性相关性，在分析时间上节省了六倍以上，溶剂消耗量节省了二十倍以上，因此在成本方面具有优势。所以，它对制药工业生产有益。
