色谱

色谱 ›› 2011, Vol. 29 ›› Issue (02): 172-175.DOI: 10.3724/SP.J.1123.2011.00172

• 技术与应用 • 上一篇    下一篇

固相萃取气相色谱-质谱法检测尿液中乙基葡萄糖醛酸苷

于天晓1,李青2,2,万涛2,2,李剑波2,2,丁世家3   

  1. 1. 重庆医科大学医学检验系, 临床检验诊断学教育部重点实验室, 重庆 400016; 2. 重庆医科大学基础医学院法医学教研室, 重庆 400016
  • 收稿日期:2010-10-19 修回日期:2011-01-05 出版日期:2011-02-28 发布日期:2007-03-25
  • 通讯作者: 丁世家,博士,教授,主要研究方向为生物分析化学
  • 基金资助:

    重庆市自然科学基金项目(No. CSTC-2007BB5314).

Determination of ethyl glucuronide in human urine by solid phase extraction-gas chromatography-mass spectrometry

YU Tianxiao1, LI Qing1, WAN Tao1, LI Jianbo2*, DING Shijia1*   

  1. 1. Department of Laboratory Medicine, Key Laboratory of Clinical Laboratory Diagnostics of Ministry of Education, Chongqing Medical University, Chongqing 400016, China; 2. Department of Forensic Medicine Science, College of Basic Medicine, Chongqing Medical University, Chongqing 400016, China
  • Received:2010-10-19 Revised:2011-01-05 Online:2011-02-28 Published:2007-03-25

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摘要： 建立了固相萃取(SPE)-气相色谱-质谱(GC-MS)检测尿液样本中乙基葡萄糖醛酸苷(EtG)的方法。1 mL尿液样本经100 μL 3 mol/L盐酸去蛋白后,通过SPE法提取上清液中的目标物质及内标,提取物经衍生化后,采用GC-MS检测,选择离子模式(SIM)扫描,内标法定量分析。该方法在0.1～3.2 mg/L范围内呈良好的线性关系,相关系数(r)为0.9921,检出限为28.4 μg/L,绝对回收率范围为92.5%～108.7%,相对标准偏差均小于5%。实验结果表明该法灵敏度高、特异性好、分析结果准确可靠,适用于法医学鉴定和临床检验中对EtG的分析测定。

关键词: 固相萃取, 气相色谱-质谱, 衍生化, 乙基葡萄糖醛酸苷

Abstract: A solid phase extraction (SPE) and gas chromatography (GC) with mass spectrometry (MS) method for determination of ethyl glucuronide (EtG) in human urine was established. One mL urine sample was deproteinated by 100 μL 3 mol/L hydrochloric acid and cleaned up through a solid phase extraction column. The target analytes were eluted from an NH2-column with 4% ammonia solution and then treated with bis(trimethylsilyl)trifluoroacetamide (BSTFA)+trimethylchlorosilane (TMCS) (99:1) for derivatization. The derivatized samples were analyzed by GC-MS. Data were acquired in the selected ion monitoring (SIM) mode and the quantitation of EtG was done through internal standard method. Good linearity was obtained at the mass concentration range of 0.1~3.2 mg/L with a correlation coefficient (r) of 0.9921. The limit of detection (LOD) was 28.4 μg/L. The range of recoveries was 92.5%~108.7%, and the relative standard deviations (RSDs) of intra-day and inter-day were all less than 5%. This method is sensitive, specific, accurate and can be applied to the determination of EtG for medicolegal identification and clinical laboratory.

Key words: derivatization, ethyl glucuronide (EtG), gas chromatography-mass spectrometry (GC-MS), solid phase extraction (SPE)