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通过阳离子交换固相萃取及液相色谱 - 串联质谱法测定尿液中用于运动药物分析的选定兴奋剂。

Determination of selected stimulants in urine for sports drug analysis by solid phase extraction via cation exchange and means of liquid chromatography-tandem mass spectrometry.

作者信息

Thomas Andreas, Sigmund Gerd, Guddat Sven, Schänzer Wilhelm, Thevis Mario

机构信息

Center for Preventive Doping Research, Institute of Biochemistry, German Sport University Cologne, Am Sportpark Müngersdorf 6, 50933 Cologne, Germany.

出版信息

Eur J Mass Spectrom (Chichester). 2008;14(3):135-43. doi: 10.1255/ejms.925.

Abstract

Stimulatory substances applied during competition possess a reasonable potential as performance enhancing agents and their misuse in elite sport has been frequently reported during the last few decades. An analytical method for the qualitative determination of selected stimulants containing a primary or secondary amine moiety in human urine for doping control purposes was developed. A rapid and highly specific procedure based on a sample preparation using weak cation exchange solid phase extraction (SPE-XCW) followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) with a C6-Phenyl analytical column allowed the unambiguous identification of the target analytes down to low ng mL(-1) concentration levels. Validation provided recovery rates of better than 75%, precisions of less than 20% and a linear approximation in the required working range (10-750 ng mL(-1)) were obtained for 19 different target compounds. This method provides a rugged and highly specific alternative to the established method utilising gas or liquid chromatography after liquid-liquid extraction.

摘要

在比赛期间使用的刺激性物质具有作为提高成绩药物的合理潜力,在过去几十年里,其在精英体育中的滥用情况屡有报道。开发了一种用于定性测定人尿中选定的含有伯胺或仲胺部分的兴奋剂的分析方法,用于兴奋剂检测。一种基于使用弱阳离子交换固相萃取(SPE-XCW)进行样品制备,随后采用带有C6-苯基分析柱的液相色谱-串联质谱(LC-MS/MS)的快速且高度特异的程序,能够明确鉴定出低至纳克每毫升(ng mL(-1))浓度水平的目标分析物。验证结果表明,19种不同目标化合物的回收率优于75%,精密度小于20%,并且在所需的工作范围(10 - 750 ng mL(-1))内获得了线性近似。该方法为采用液液萃取后进行气相或液相色谱分析的既定方法提供了一种耐用且高度特异的替代方法。

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