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液相色谱-串联质谱法同时测定人血浆中二甲双胍和西他列汀的方法开发与验证及其在生物等效性研究中的应用

Development and Validation of a Method for Simultaneous Estimation of Metformin and Sitagliptin in Human Plasma by LC-MS-MS and Its Application in a Bioequivalence Study.

作者信息

Reddy Srinivasa, Ahmed Imran, Ahmad Iqbal, Mukhopadhyay Arindam, Thangam Saral

机构信息

Norwich Clinical Services Pvt Ltd, 147/F, 8th Main, 3rd Block, Koramangala, Bangalore 560034, India.

Norwich Clinical Services Pvt Ltd, 147/F, 8th Main, 3rd Block, Koramangala, Bangalore 560034, India

出版信息

J Chromatogr Sci. 2015 Oct;53(9):1549-56. doi: 10.1093/chromsci/bmv055. Epub 2015 May 17.

DOI:10.1093/chromsci/bmv055
PMID:25987553
Abstract

A simple, sensitive, precise and accurate method for simultaneous estimation of metformin and sitagliptin from human plasma was developed and validated. Samples extracted from plasma using acetonitrile were separated on an SCX column and estimated using API 4000 Mass Spectrometer in the positive atmospheric pressure ionization mode (Turboionspray) by following multiple reaction monitoring transitions for both parent and daughter ions. A linear calibration plot was achieved for both the analytes in the concentration ranges of 10-2,206 ng/mL (for metformin) and 3-800.5 ng/mL (for sitagliptin) prepared in K2EDTA pooled plasma. Mean recovery for metformin was 92% and for sitagliptin was 104.5%. It is a fully validated method and successfully applied for estimation of these drug molecules during biostudies.

摘要

开发并验证了一种从人血浆中同时测定二甲双胍和西他列汀的简单、灵敏、精确且准确的方法。使用乙腈从血浆中提取的样品在强阳离子交换柱上进行分离,并通过在正大气压电离模式(Turboionspray)下使用API 4000质谱仪,对母离子和子离子进行多反应监测转换来进行测定。在K2EDTA混合血浆中制备的浓度范围为10 - 2,206 ng/mL(二甲双胍)和3 - 800.5 ng/mL(西他列汀)内,两种分析物均获得了线性校准曲线。二甲双胍的平均回收率为92%,西他列汀的平均回收率为104.5%。这是一种经过充分验证的方法,并成功应用于生物研究中这些药物分子的测定。

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