Mazzarino Monica, Botrè Francesco
Laboratorio Antidoping, Federazione Medico Sportiva Italiana, Largo Giulio Onesti 1, 00197 Rome, Italy.
Rapid Commun Mass Spectrom. 2006;20(22):3465-76. doi: 10.1002/rcm.2729.
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.
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。