Polagani Srinivasa Rao, Pilli Nageswara Rao, Gandu Venkateswarlu
Research Studies, Rayalaseema University, Kurnool 518 002, India.
University College of Pharmaceutical Sciences, Jawaharlal Nehru Technological University, Kukatpally, Hyderabad 500 085, India.
J Pharm Anal. 2012 Jun;2(3):206-213. doi: 10.1016/j.jpha.2012.01.001. Epub 2012 Feb 4.
A rapid and sensitive liquid chromatography-tandem mass spectrometric (LC-MS/MS) assay method has been developed and fully validated for the simultaneous quantification of pravastatin and aspirin in human plasma. Furosemide was used as an internal standard. Analytes and the internal standard were extracted from human plasma by liquid-liquid extraction technique using methyl tertiary butyl ether. The reconstituted samples were chromatographed on a Zorbax SB-C column by using a mixture of 5 mM ammonium acetate buffer and acetonitrile (20:80, v/v) as the mobile phase at a flow rate of 0.8 mL/min. The calibration curve obtained was linear (≥0.99) over the concentration range of 0.50-600.29 ng/mL for pravastatin and 20.07-2012.00 ng/mL for aspirin. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. A run time of 2.0 min for each sample made it possible to analyze more than 400 human plasma samples per day. The proposed method was found to be applicable to clinical studies.
已开发并完全验证了一种快速灵敏的液相色谱 - 串联质谱（LC-MS/MS）分析方法，用于同时定量人血浆中的普伐他汀和阿司匹林。呋塞米用作内标。采用甲基叔丁基醚通过液 - 液萃取技术从人血浆中提取分析物和内标。将重构后的样品在Zorbax SB-C柱上进行色谱分析，以5 mM醋酸铵缓冲液和乙腈（20:80，v/v）的混合物作为流动相，流速为0.8 mL/min。获得的校准曲线在普伐他汀浓度范围为0.50 - 600.29 ng/mL和阿司匹林浓度范围为20.07 - 2012.00 ng/mL内呈线性（≥0.99）。按照FDA指南进行方法验证，结果符合验收标准。每个样品的运行时间为2.0分钟，使得每天能够分析400多个人类血浆样品。该方法被发现适用于临床研究。
