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[液相色谱-质谱法测定三种合成代谢类固醇]

[Determination of three anabolic steroids by liquid chromatography-mass spectrometry].

作者信息

Qin Yang, Liu Xin, Wang Zhanliang, Wu Moutian

机构信息

China Anti-Doping Agency, General Administration of Sport of China, Beijing 100029, China.

出版信息

Se Pu. 2008 Jul;26(4):465-8.

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 beta-glucuronidase, then extracted with methyl tert-butyl ether. Chromatographic separation was performed on a Zorbax SB-C18 column (150 mm x 2.1 mm, 5 microm) 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.

摘要

建立了一种高效液相色谱 - 电喷雾电离质谱法(LC - ESI/MS)用于筛查和测定人尿中的群勃龙、四氢孕三烯酮和孕三烯酮。尿样用β - 葡萄糖醛酸酶进行酶解,然后用甲基叔丁基醚萃取。采用Zorbax SB - C18柱(150 mm×2.1 mm,5微米),以甲酸铵缓冲液(pH 3.5)和乙腈为流动相进行色谱分离。采用正电喷雾电离模式,研究了电喷雾室不同参数的影响。基于信噪比为3的检测限在1至5纳克之间。该方法可应用于兴奋剂检测中合成代谢类固醇的筛查和确证。

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