Kumar P Pavan, Murthy T E G K, Basaveswara Rao M V
Department of Pharmaceutical Sciences, Krishna University, Machilipatnam, India.
Department of Pharmaceutics, Bapatla College of Pharmacy, Bapatla, Guntur, Andhra Pradesh, India.
J Adv Pharm Technol Res. 2015 Jul-Sep;6(3):118-24. doi: 10.4103/2231-4040.157982.
A new, simple and accurate liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for simultaneous determination of rosuvastatin (ROS) and metformin (MET) in human plasma was developed. The assay procedure involved simple protein precipitation with acetonitrile. Following precipitation, fraction of supernatant was decanted and evaporated under gentle stream of nitrogen at 40°C. The residue was reconstituted in mobile phase and injected. The chromatographic separation was achieved with Thermo Hypurity C18 column (50 mm × 4.6 mm, 5 μ) using a mobile phase composition containing 0.1% v/v formic acid in water and acetonitrile (30:70, v/v) at a flow rate of 0.4 mL/min. The total run time was 3.5 min. The method showed good linearity in the range 0.5-200 ng/mL for ROS and 2-2000 ng/mL for MET with correlation coefficient (r) >0.9994 for both the analytes. The intra and inter-day precision values for ROS and MET met the acceptance criteria as per regulatory guidelines. The battery of stability studies viz., bench-top, freeze-thaw and long term stability were performed. The developed method was applied to a pharmacokinetic study.
建立了一种新的、简单且准确的液相色谱-串联质谱（LC-MS/MS）法，用于同时测定人血浆中的瑞舒伐他汀（ROS）和二甲双胍（MET）。测定步骤包括用乙腈进行简单的蛋白沉淀。沉淀后，倾析出上清液部分，并在40℃的氮气流下蒸发。残留物用流动相复溶并进样。使用Thermo Hypurity C18柱（50 mm×4.6 mm，5μm）进行色谱分离，流动相组成为含0.1% v/v甲酸的水和乙腈（30:70，v/v），流速为0.4 mL/min。总运行时间为3.5分钟。该方法在ROS浓度范围为0.5 - 200 ng/mL、MET浓度范围为2 - 2000 ng/mL时显示出良好的线性，两种分析物的相关系数（r）均>0.9994。ROS和MET的日内和日间精密度值符合监管指南的接受标准。进行了一系列稳定性研究，即台式稳定性、冻融稳定性和长期稳定性研究。所建立的方法应用于一项药代动力学研究。
