Razzaq Syed Naeem, Khan Islam Ullah, Mariam Irfana, Razzaq Syed Saleem
Department of Chemistry, Government College University, Lahore, 54000, Pakistan.
Chem Cent J. 2012 Sep 4;6(1):94. doi: 10.1186/1752-153X-6-94.
A simple, specific, and fast stability indicating reverse phase liquid chromatographic method was established for instantaneous determination of moxifloxacin and prednisolone in bulk drugs and pharmaceutical formulations.
Optimum chromatographic separations among the moxifloxacin, prednisolone and stress-induced degradation products were achieved within 10 minutes by use of BDS Hypersil C8 column (250 X 4.6 mm, 5 μm) as stationary phase with mobile phase consisted of a mixture of phosphate buffer (18 mM) containing 0.1% (v/v) triethylamine, at pH 2.8 (adjusted with dilute phosphoric acid) and methanol (38:62 v/v) at a flow rate of 1.5 mL min-1. Detection was performed at 254 nm using diode array detector. The method was validated in accordance with ICH guidelines. Response was a linear function of concentrations over the range of 20-80 μg mL-1 for moxifloxacin (r2 ≥ 0.998) and 40-160 μg mL-1 for prednisolone (r2 ≥ 0.998). The method was resulted in good separation of both the analytes and degradation products with acceptable tailing and resolution. The peak purity index for both the analytes after all types of stress conditions was ≥ 0.9999 indicated a complete separation of both the analyte peaks from degradation products. The method can therefore, be regarded as stabilityindicating.
The developed method can be applied successfully for simultaneous determination of moxifloxacin and prednisolone in pharmaceutical formulations and their stability studies.
建立了一种简单、特异且快速的反相液相色谱稳定性指示方法，用于原料药和药物制剂中莫西沙星和泼尼松龙的即时测定。
使用BDS Hypersil C8柱（250×4.6 mm，5μm）作为固定相，流动相由含0.1%（v/v）三乙胺的磷酸盐缓冲液（18 mM）（用稀磷酸调至pH 2.8）和甲醇（38:62 v/v）的混合物组成，流速为1.5 mL min-1，在10分钟内实现了莫西沙星、泼尼松龙及其应激诱导降解产物的最佳色谱分离。使用二极管阵列检测器在254 nm处进行检测。该方法按照ICH指南进行了验证。莫西沙星在20 - 80μg mL-1浓度范围内响应呈线性函数（r2≥0.998），泼尼松龙在40 - 160μg mL-1浓度范围内响应呈线性函数（r2≥0.998）。该方法对两种分析物和降解产物均实现了良好分离，拖尾和分离度均可接受。所有应激条件下两种分析物的峰纯度指数均≥0.9999，表明分析物峰与降解产物完全分离。因此，该方法可被视为稳定性指示方法。
所建立的方法可成功应用于药物制剂中莫西沙星和泼尼松龙的同时测定及其稳定性研究。
