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一种用于同时检测合成糖皮质激素、某些兴奋剂、抗雌激素药物和合成代谢类固醇的快速液相色谱/质谱筛查方法。

A fast liquid chromatographic/mass spectrometric screening method for the simultaneous detection of synthetic glucocorticoids, some stimulants, anti-oestrogen drugs and synthetic anabolic steroids.

作者信息

Mazzarino Monica, Botrè Francesco

机构信息

Laboratorio Antidoping, Federazione Medico Sportiva Italiana, Largo Giulio Onesti 1, 00197 Rome, Italy.

出版信息

Rapid Commun Mass Spectrom. 2006;20(22):3465-76. doi: 10.1002/rcm.2729.

Abstract

A fast liquid chromatographic/mass spectrometric (LC/MS/MS) screening method for the detection, in urine, of synthetic glucocorticoids, stimulants (formoterol, modafinil and mesocarb), anti-oestrogens (finasteride, exemestane, anastrozole, letrozole and formestane) and synthetic anabolic steroids (stanozolol, gestrinone and tetrahydrogestrinone) is described. All these drugs (and/or their urinary metabolites) can be simultaneously extracted by a single liquid/liquid extraction step, at alkaline pH, after enzymatic hydrolysis with beta-glucuronidase, and assayed in 7 min by LC/MS/MS using electrospray ionization in positive ion mode and multiple reaction monitoring as the acquisition mode. All compounds show good reproducibility of both the retention times (CV% <2%) and the relative abundances (CV% <10%). The limits of detection for the anti-oestrogens, glucocorticoids and steroids are in the range of 1-30 ng/mL, and for the stimulants are in the range of 100-200 ng/mL, thus satisfying the minimum required performance limits of the World Anti-Doping Agency.

摘要

描述了一种快速液相色谱/质谱联用(LC/MS/MS)筛查方法,用于检测尿液中的合成糖皮质激素、兴奋剂(福莫特罗、莫达非尼和美索卡)、抗雌激素(非那雄胺、依西美坦、阿那曲唑、来曲唑和福美坦)以及合成代谢类固醇(司坦唑醇、孕三烯酮和四氢孕三烯酮)。所有这些药物(和/或其尿液代谢物)在经β-葡萄糖醛酸酶进行酶水解后,于碱性pH条件下通过单步液液萃取同时提取,并在7分钟内通过LC/MS/MS进行测定,采用正离子模式下的电喷雾电离和多反应监测作为采集模式。所有化合物的保留时间(CV%<2%)和相对丰度(CV%<10%)均具有良好的重现性。抗雌激素、糖皮质激素和类固醇的检测限在1 - 30 ng/mL范围内,兴奋剂的检测限在100 - 200 ng/mL范围内,从而满足了世界反兴奋剂机构规定的最低性能要求限值。

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