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使用液相色谱-串联质谱法对人血浆中新型β₂肾上腺素能受体激动剂川丁特罗进行快速灵敏的检测。

Rapid and sensitive assay for trantinterol, a novel beta(2)-adrenoceptor agonist, in human plasma using liquid chromatography-tandem mass spectrometry.

作者信息

Sun Yantong, Liu Mingyuan, Zhang Jiwen, Jiang Yao, Yu Weisong, Fawcett John Paul, Gu Jingkai

机构信息

Research Center for Drug Metabolism, College of Life Science, Jilin University, Changchun, China.

出版信息

J Pharm Biomed Anal. 2009 May 1;49(4):1056-9. doi: 10.1016/j.jpba.2009.01.012. Epub 2009 Jan 20.

Abstract

A rapid and sensitive assay for trantinterol, a novel beta(2)-adrenoceptor agonist, in human plasma has been developed. Samples containing the analyte and internal standard, clenbuterol, were analyzed by liquid chromatography-tandem mass spectrometry after liquid-liquid extraction with diethyl ether:dichloromethane (60:40, v/v). Separation was performed on a Venusil MP C(18) column (50 mm x 4.6 mm, 5 microm) using methanol:1% formic acid (50:50, v/v) as mobile phase and monitored by multiple reaction monitoring of the precursor-to-product ion transitions of trantinterol at m/z 311.2-->238.1 and clenbuterol at m/z 277.2 --> 203.1. The total run time was only 1.5 min and the method was linear over the concentration range 1-1000 pg/mL with a lower limit of quantitation of 1 pg/mL. Intra- and inter-day precisions (relative standard deviation) were below 7% and 12%, respectively, with accuracy (relative error) below 8%. The method was successfully applied to a pharmacokinetic study involving oral administration of a 50 microg trantinterol tablet to healthy volunteers.

摘要

已开发出一种用于检测人血浆中新型β₂肾上腺素能受体激动剂川丁特罗的快速灵敏分析方法。含有分析物和内标克伦特罗的样品,经乙醚:二氯甲烷(60:40,v/v)液液萃取后,采用液相色谱-串联质谱法进行分析。在Venusil MP C₁₈柱(50 mm×4.6 mm,5 µm)上进行分离,以甲醇:1%甲酸(50:50,v/v)作为流动相,并通过对川丁特罗m/z 311.2→238.1和克伦特罗m/z 277.2→203.1的前体离子到产物离子跃迁进行多反应监测来进行检测。总运行时间仅为1.5分钟,该方法在1 - 1000 pg/mL的浓度范围内呈线性,定量下限为1 pg/mL。日内和日间精密度(相对标准偏差)分别低于7%和12%,准确度(相对误差)低于8%。该方法已成功应用于一项药代动力学研究,该研究涉及对健康志愿者口服50微克川丁特罗片剂。

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