色谱

色谱

• 兴奋剂检测方法专栏 • 上一篇    下一篇

头发中内源性类固醇激素的气相色谱-串联质谱分析

沈敏,向平,沈保华,王萌烨   

  1. Institute of Forensic Sciences, Ministry of Justice, Shanghai Key Laboratory of Forensic Medicine, Shanghai 200063, 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: 沈敏
  • 基金资助:
    国家自然科学基金资助项目（编号: 20475037）

Determination of endogenous anabolic steroids in hair using gas chromatography-tandem mass spectrometry

SHEN Min, XIANG Ping, SHEN Baohua, WANG Mengye   

  1. Institute of Forensic Sciences, Ministry of Justice, Shanghai Key Laboratory of Forensic Medicine, Shanghai 200063, China
  • Received:2008-01-05 Revised:2008-07-30 Online:2008-07-30 Published:1983-12-25
  • Contact: SHEN Min

PDF

1199

被引次数

12

摘要： 建立了建康人头发中内源性类固醇兴奋剂睾酮、表睾酮、雄酮、苯胆烷醇酮和脱氢表雄酮的气相色谱-串联质谱(GC-MS/MS)分析方法。头发经碱水解后,以乙醚提取，经衍生化后采用GC-MS/MS的多反应监测模式(MRM)分析。方法的线性关系良好,检出限达0.1～0.2 pg/mg；提取回收率为74.6%～104.5%；日内测定的准确度为90.1%～113.7%,日内及日间测定的精密度均小于17.5%。应用所建立的方法测定了80例中国健康人头发中睾酮、表睾酮、雄酮、苯胆烷醇酮和脱氢表雄酮的生理水平,为内源性类固醇兴奋剂滥用的判断提供了方法和基础数据。

关键词: 毛发 , 内源性类固醇激素, 气相色谱-串联质谱

Abstract: A method of gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed for the simultaneous identification and quantification of five endogenous anabolic steroids (testosterone, epitestosterone, androsterone, etiocholanolone, dehydroepiandrosterone) in hair. After alkaline hydrolysis, the hair sample was extracted with diethyl ether, derivatized with a derivatization reagent (N-methyl-N-trimethylsilyl-trifluoroacetamid/iodotrimethyisilane/DL-dithiothreitol, 1000∶5∶5, v/v/w) and detected using GC-MS/MS in the multiple-reaction monitoring mode. The one precursor/two product ion transitions for each anabolic steroids were monitored. The limits of detection for five endogenous anabolic steroids were in the range of 0.1-0.2 pg/mg. All analytes showed good linearity and the extraction recoveries were 74.6%-104.5%. The inter-day and intra-day relative standard deviations （RSD） were less than 17.5%. This method has been applied to the analysis of testosterone, epitestosterone, androsterone, etiocholanolone, dehydroepiandrosterone in 80 Chinese hair samples. These data are the suitable references and the basis for the interpretation of the results from endogenous steroids abuse.

Key words: endogenous steroids, hair , gas chromatography-tandem mass spectrometry （GC-MS/MS）