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.