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采用液相色谱-质谱联用技术测定人血浆中氯吡格雷代谢物(SR26334)的含量。

Determination of clopidogrel metabolite (SR26334) in human plasma by LC-MS.

作者信息

Ksycinska Hanna, Rudzki Piotr, Bukowska-Kiliszek Mirosława

机构信息

Department of Pharmacology, Pharmaceutical Research Institute, 8 Rydygiera Street, 01-793 Warsaw, Poland.

出版信息

J Pharm Biomed Anal. 2006 May 3;41(2):533-9. doi: 10.1016/j.jpba.2005.11.035. Epub 2006 Jan 6.

DOI:10.1016/j.jpba.2005.11.035
PMID:16406450
Abstract

A new, sensitive, specific and reproducible method for determination of clopidogrel metabolite (SR26334) in human plasma has been developed. After liquid-liquid extraction on Chem Elut cartridges with dichloromethane, samples were quantified using reversed-phase high performance liquid chromatography with mass detection. The determination was performed on a Luna C18, 3 microm (75 mmx4.6 mm i.d.) column with an acetonitrile-water-formic acid mixture (60:40:0.1, v/v/v) as a mobile phase. The flow rate was set at 0.2 mL/min. Repaglinide was chosen as an internal standard and the time of analysis was 12 min. For SR26334 the limits of detection and quantification were 7.5 ng/mL and 20 ng/mL, respectively, and the calibration curve was linear up to 3000 ng/mL. The extraction recovery of SR26334 from plasma was within the range of 85-90%. The method has been successfully used to study clopidogrel metabolite pharmacokinetics in healthy volunteers.

摘要

已开发出一种用于测定人血浆中氯吡格雷代谢物(SR26334)的新的、灵敏、特异且可重复的方法。使用二氯甲烷在Chem Elut柱上进行液 - 液萃取后,采用反相高效液相色谱 - 质谱检测对样品进行定量。测定在Luna C18,3微米(75毫米×4.6毫米内径)柱上进行,以乙腈 - 水 - 甲酸混合物(60:40:0.1,v/v/v)作为流动相。流速设定为0.2毫升/分钟。选择瑞格列奈作为内标,分析时间为12分钟。对于SR26334,检测限和定量限分别为7.5纳克/毫升和20纳克/毫升,校准曲线在高达3000纳克/毫升范围内呈线性。SR26334从血浆中的萃取回收率在85 - 90%范围内。该方法已成功用于研究健康志愿者体内氯吡格雷代谢物的药代动力学。

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