液相色谱-电喷雾电离质谱法检测尿液中的3种合成类固醇药物  

Determination of three anabolic steroids by liquid chromatography-mass spectrometry

作　　者：秦旸[1] 刘欣[1] 王占良[1] 吴侔天[1] 

机构地区：[1]国家体育总局中国反兴奋剂中心,北京100029

出　　处：《色谱》2008年第4期465-468,共4页Chinese Journal of Chromatography

基　　金：国家自然科学基金资助项目(No.20635001)

摘　　要：研究建立了合成类固醇药物群勃龙、四氢孕三烯炔酮和孕三烯酮的液相色谱-电喷雾质谱的检测方法。尿样经过β-葡萄糖醛酸酶酶解和叔丁基甲醚提取后,采用Zorbax SB-C18分析柱(150mm×2.1mm,5μm),在流动相为pH3.5的甲酸铵缓冲液-乙腈的条件下进行梯度洗脱,在正离子模式下检测。考察了不同的质谱条件对这类化合物检测结果的影响。建立了人尿液中合成类固醇药物的液相色谱-电喷雾电离质谱的初筛和确证方法。A high performance liquid chromatography-electrospray ionization mass spectrometry （LC-ESI/MS） was developed to screen and determine trenbolone, tetrahydrogestrinone and gestrinone in human urine. The urine sample was enzymaticaUy hydrolyzed with β-glucuronidase, then extracted with methyl tert-butyl ether. Chromatographic separation was performed on a Zorbax SB-C18 column （150 mm × 2.1mm, 5 μm） with ammonium formate buffer （pH 3.5 ） and acetonitrile as mobile phase. Using positive electrospray ionization mode, the effect of different parameters from electrospray chamber was investigated. The limits of detection based on signal noise ratio of 3 were between 1 and 5 ng. The method can be applied in screening and confirmation of the anabolic steroids in doping control.

关 键 词：液相色谱-电喷雾电离质谱 合成类固醇 人尿液 兴奋剂检测 

分 类 号：O658[理学—分析化学]