色谱

色谱

• 兴奋剂检测方法专栏 • 上一篇    下一篇

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

秦旸,刘欣,王占良,吴侔天   

  1. China Anti-Doping Agency, General Administration of Sport of China, Beijing 100029, China
  • 收稿日期:2008-01-05 修回日期:2008-07-30 出版日期:2008-07-30 发布日期:1983-12-25
  • 通讯作者: 秦旸
  • 基金资助:
    国家自然科学基金资助项目(No. 20635001)

Determination of three anabolic steroids by liquid chromatography-mass spectrometry

QIN Yang, LIU Xin, WANG Zhanliang, WU Moutian   

  1. China Anti-Doping Agency, General Administration of Sport of China, Beijing 100029, China
  • Received:2008-01-05 Revised:2008-07-30 Online:2008-07-30 Published:1983-12-25
  • Contact: QIN Yang

PDF

1105

被引次数

7

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(150 mm×2.1 mm,5 μm),在流动相为pH 3.5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。

关键词: 合成类固醇, 人尿液, 兴奋剂检测 , 液相色谱-电喷雾电离质谱

Abstract: 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 enzymatically hydrolyzed with β-glucuronidase, then extracted with methyl tert-butyl ether. Chromatographic separation was performed on a Zorbax SB-C18 column (150 mm×2.1 mm, 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.

Key words: anabolic steroids, doping detection , human urine, liquid chromatography-electrospray ionization mass spectrometry (LC-ESI/MS)