Simultaneous estimation of rosuvastatin and amlodipine in pharmaceutical formulations using stability indicating HPLC method

A viable cost-effective and isocratic approach employing C-18 column (250 mm × 4.6 mm, 5 µm) based HPLC has been utilized to separate and estimate the drugs, rosuvastatin, amlodipine and their stress induced degradation products, simultaneously in pharmaceutical formulations. Focused on ICH guideline parameters, the efficient separation of both drugs and their degradation products was achieved by optimizing a 30:70 (v/v) solvent mixture of acetonitrile and 0.1 M ammonium acetate buffer (pH 5) as mobile phase. The flow rate of the mobile phase was 1.5 mL/min and all the detections were carried out at 240 nm using UV detector. The method was linear in the concentration range of 1-200 µg/mL for rosuvastatin with 0.996 coefficient of determination value. For amlodipine, linearity was in the range of 0.5-100 µg/ml with 0.994 coefficient of determination value. Both the drugs along with their degradation products were separated in less than twenty minutes. The results of within-day and between-day precision were varied from 0.72 to 1.81% for rosuvastatin and 0.83 to 1.88% for amlodipine. The results show that this ICH validated method can be employed successfully for the routine as well as stability quantification of both the active ingredients simultaneously in pharmaceutical formulations.

本研究建立了一种经济可行的等度高效液相色谱(HPLC)分析方法，采用规格为250 mm × 4.6 mm、粒径5 µm的C-18色谱柱(C-18 column)，可同时分离并定量药物制剂中的瑞舒伐他汀(rosuvastatin)、氨氯地平(amlodipine)及其强制降解产物。本方法遵循国际人用药品注册技术协调会(ICH, International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use)指南的参数要求，通过优化以乙腈(acetonitrile)与0.1 M醋酸铵缓冲液(ammonium acetate buffer，pH 5)按30:70体积比组成的流动相，实现了两种药物及其降解产物的高效分离。流动相流速设定为1.5 mL/min，所有检测均采用紫外检测器(UV detector)在240 nm波长下完成。瑞舒伐他汀在1~200 µg/mL浓度范围内呈良好线性关系，决定系数为0.996；氨氯地平的线性范围为0.5~100 µg/mL，决定系数为0.994。两种药物及其降解产物均可在20分钟内完成分离。日内及日间精密度的测定结果显示，瑞舒伐他汀的相对偏差介于0.72%~1.81%之间，氨氯地平则介于0.83%~1.88%之间。研究结果表明，经ICH验证的该方法可成功用于药物制剂中两种活性成分的常规定量分析与稳定性定量检测，且可同时完成相关测定。