色谱

色谱

• 兴奋剂检测方法专栏 • 上一篇    下一篇

气相色谱-质谱联用技术用于尿样中β-阻断剂的初筛定量和确证

上官良敏,刘薇,郑向阳,张兰   

  1. Key Laboratory of Analysis and Detection for Food Safety, Ministry of Education, Sport Science Research Center, Fuzhou University, Fuzhou 350002, 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: 张兰
  • 基金资助:
    福建省体育局重大专项、福建省自然科学基金(B0510006, 2007J0279)、福建省教育厅科技计划项目(2007F5067)、福建省科技厅国际合作重点项目（2007I0020）、福建省科技厅重点项目(2007Y0060)和福建省高校新世纪优秀人才支持计划资助.

Screening, quantification and confirmation of β-blockers in urine using gas chromatography-mass spectrometry

SHANGGUAN Liangmin, LIU Wei, ZHENG Xiangyang, ZHANG Lan   

  1. Key Laboratory of Analysis and Detection for Food Safety, Ministry of Education, Sport Science Research Center, Fuzhou University, Fuzhou 350002, China
  • Received:2008-01-05 Revised:2008-07-30 Online:2008-07-30 Published:1983-12-25
  • Contact: ZHANG Lan

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1060

被引次数

4

摘要： 建立了一种同时测定5种β-阻断剂(卡替洛尔、艾司洛尔、普萘洛尔、索他洛尔、比索洛尔)的气相色谱-质谱方法(GC-MS),并用于疑似阳性实际尿样的初筛、定量和确证。分别对游离态和结合态药物进行了提取,合并提取液后采用N-甲基-N-三甲基硅基-三氟乙酰胺(C6H12F3NOSi, MSTFA)和N-甲基-双三氟乙酰胺试剂(C5H3F6NO2, MBTFA)进行混合衍生。确定了优化的GC-MS条件,建立了采用选择离子监测方式（SIM）初筛和全扫描方式（SCAN）确证的实验流程;建立了SIM模式下5种β-阻断剂的尿样加标工作曲线,其SIM方法的检出限达0.2～1.0 ng/mL,尿样的加标回收率为70.5%～103.4%,相对标准偏差小于14.9%。该方法成功地用于普萘洛尔阳性尿样的检测,并绘制了普萘洛尔的尿代谢曲线。该方法对兴奋剂检测中β-阻断剂滥用的控制有重要的意义。

关键词: β-阻断剂, 尿液 , 气相色谱-质谱, 兴奋剂检测

Abstract: A method was developed to perform the screening, quantification and confirmation of the five β-blockers, propranolol, carteolol, bisoprolol, esmolol, and sotalol, in human urine using gas chromatography-mass spectrometry (GC-MS). In sample preparation, conjugated and unconjugated β-blockers in urine were extracted separately, and the extracts were combined. The extracts were derivatized with N-methyl-N-trimethylsilyl-trifluoroacetamide （MSTFA） and N-methyl-bis(trifluoroacetamide) （MBTFA）. The optimal conditions of GC-MS were established, and the progresses of screening by selected ion monitoring (SIM) mode and confirmation by full scan (SCAN) mode were completed. At last, the quantification curves of the five β-blockers in spiked urine were established by SIM mode. The limits of detection were 0.2-1.0 ng/mL. Overall recoveries were 70.5%-103.4%, and the relative standard deviations were lower than 15%. In addition, the method was successfully applied to the analysis of the positive urine of propranolol, and the urinary excretion curve was also established accordingly. It is significant to prohibit the abuse of β-blockers in doping control.

Key words: doping detection, urine , β-blockers, gas chromatography-mass spectrometry (GC-MS)