色谱

• 兴奋剂检测方法专栏 • 上一篇    下一篇

液相色谱-串联质谱法测定毛发中的司坦唑醇

向平,沈敏,沈保华,严慧   

  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: 向平
  • 基金资助:
    国家自然科学基金项目(编号:20475037)和上海自然科学基金项目(编号:07ZR14114)资助.

Determination of stanozolol in hair using liquid chromatography-tandem mass spectrometry

XIANG Ping, SHEN Min, SHEN Baohua, YAN Hui   

  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: XIANG Ping

摘要: 采用液相色谱-串联质谱(LC-MS/MS)建立了毛发中司坦唑醇的分析方法,并将其应用于单次给药动物实验中的动物毛样品分析。将10 mg样品碱水解后加入戊烷提取,然后进行LC-MS/MS分析,采用正离子电喷雾电离、多反应监测模式测定,方法的最低定量限为25 pg/mg。剃去豚鼠背部中央的毛,以60 mg/kg的剂量于豚鼠腹腔注射司坦唑醇,然后隔天在同一部位剃取其毛,两周内该豚鼠毛中均能检出司坦唑醇;给药后豚鼠毛中司坦唑醇的含量在第1周内保持稳定,在给药后第10天达到峰值。所建立的方法毛发取样量少,特异性强,灵敏度高,适用于毛发中司坦唑醇的分析。

关键词: 毛发 , 司坦唑醇, 液相色谱-串联质谱

Abstract: A rapid and sensitive method was developed for the identification and quantification of stanozolol in hair. After alkaline hydrolysis, the hair sample (10 mg) was extracted with pentane, and analyzed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) with electrospray ionization (ESI) and multiple reaction monitoring (MRM). The limit of quantification was found to be 25 pg/mg. After shaving hair on the back of the cavies, they were received after a single intraperitoneal dosing of stanozolol of 60 mg/kg. The hair segments were shaved once every two days for two weeks. The concentration of stanozolol in segmented hair reached the highest at the 10th day. The features of the method are of small sample size, specific, sensitive and suitable for the determination of stanozolol in hair.

Key words: hair , stanozolol, liquid chromatography-tandem mass spectrometry (LC-MS/MS)