Van Thuyne W, Van Eenoo P, Delbeke F T
DoCoLab - UGent, Department of Clinical Chemistry, Microbiology and Immunology, Technologiepark 30, B-9052 Zwijnaarde, Belgium.
J Chromatogr A. 2008 Nov 14;1210(2):193-202. doi: 10.1016/j.chroma.2008.09.049. Epub 2008 Sep 19.
A comprehensive screening method for the detection of prohibited substances in doping control is described and validated. This method is capable of detecting over 150 components mentioned on the list of the World Anti-Doping Agency including anabolic androgenic steroids, stimulants and all narcotic agents that are currently analysed using different analytical methods. The analytes are extracted from urine by a combined extraction procedure using freshly distilled diethyl ether and tert-butyl methyl ether as extraction solvents at pH 9.5 and 14 respectively. Prior to GC-MS analysis the residues are combined and derivatised using a mixture of N-methyl-N-trimethylsilyltrifluoroacetamide, NH(4)I and ethanethiol. The mass spectrometer is simultaneously operated in the full scan mode (mass range varies along with GC-oven temperature program) and in the selected ion monitoring mode. The obtained limits of detection are in compliance with the requirements set by the World Anti-Doping Agency. Besides narcotics, stimulants and anabolic androgenic agents, this method is also capable of detecting several agents with anti-estrogenic activity and some beta-agonists. This comprehensive screening method reduces the amount of urine needed and increases the sample throughput without a loss in sensitivity and selectivity.
描述并验证了一种用于兴奋剂检测中违禁物质检测的综合筛选方法。该方法能够检测世界反兴奋剂机构清单上提及的150多种成分，包括合成代谢雄性类固醇、兴奋剂以及目前使用不同分析方法进行分析的所有麻醉剂。分析物通过联合萃取程序从尿液中提取，分别使用新鲜蒸馏的乙醚和叔丁基甲基醚作为萃取溶剂，pH值分别为9.5和14。在进行气相色谱-质谱分析之前，将残留物合并并用N-甲基-N-三甲基硅烷基三氟乙酰胺、NH(4)I和乙硫醇的混合物进行衍生化。质谱仪同时在全扫描模式（质量范围随气相色谱柱温程序变化）和选择离子监测模式下运行。获得的检测限符合世界反兴奋剂机构设定的要求。除了麻醉剂、兴奋剂和合成代谢雄性激素外，该方法还能够检测几种具有抗雌激素活性的药物和一些β-激动剂。这种综合筛选方法减少了所需尿液的量，提高了样品通量，同时不损失灵敏度和选择性。
