色谱

色谱 ›› 2018, Vol. 36 ›› Issue (10): 1067-1072.DOI: 10.3724/SP.J.1123.2018.05022

• 技术与应用 • 上一篇    

基于可变亲水性溶剂的液液微萃取-气相色谱-质谱法分析尿中的2'-氯地西泮

徐仿敏1, 李海波2, 魏万里3, 刘凌云1, 李强2   

  1. 1. 江阴市公安局物证鉴定室, 江苏 江阴 214431;
    2. 常州市公安局物证鉴定所, 江苏 常州 213001;
    3. 无锡市公安局物证鉴定所, 江苏 无锡 214001
  • 收稿日期:2018-06-04 出版日期:2018-10-08 发布日期:2014-08-22
  • 通讯作者: 徐仿敏,E-mail:xufangmin2003@163.com

Solvent with switchable hydrophilicity used in liquid-liquid microextraction combined with gas chromatography-mass spectrometry for the determination of diclazepam in urine

XU Fangmin1, LI Haibo2, WEI Wanli3, LIU Lingyun1, LI Qiang2   

  1. 1. Institute of Forensic Science, Public Security Bureau of Jiangyin, Jiangyin 214431, China;
    2. Institute of Forensic Science, Public Security Bureau of Changzhou, Changzhou 213001, China;
    3. Institute of Forensic Science, Public Security Bureau of Wuxi, Wuxi 214001, China
  • Received:2018-06-04 Online:2018-10-08 Published:2014-08-22

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摘要：

建立一种基于可变亲水性溶剂的液液微萃取-气相色谱-质谱联用法，快速检测尿液中2'-氯地西泮。对影响萃取效率的可变亲水性溶剂的种类、用量、转换条件、萃取时间等因素进行考察和优化。在最佳实验条件下，尿液中2'-氯地西泮的线性范围为0.025~2.5 mg/L，检出限为0.007 mg/L，日内和日间回收率为76.5%~90.3%，日内和日间精密度为3.3%~6.5%。该方法具有良好的线性、检出限、回收率和精密度，有较好的应用价值，可应用于尿液中2'-氯地西泮的分析。

关键词: 2'-氯地西泮, 可变亲水性溶剂, 尿, 气相色谱-质谱法, 液液微萃取

Abstract:

A simple, fast, and sensitive method was developed for the determination of diclazepam in urine using a solvent with switchable hydrophilicity in liquid-liquid microextraction followed by gas chromatography-mass spectrometry. N,N-Dimethylcyclohexylamine was used as the extraction solvent with switchable hydrophilicity, because it can be made miscible or immiscible with aqueous phase by adding hydrochloric acid and sodium hydroxide. Experimental parameters affecting the extraction efficiency, such as the volume of hydrochloric acid, the type and volume of the solvent with switchable hydrophilicity, the volume of sodium hydroxide, and the extraction time, were investigated. Under the optimal conditions, the intraday and interday recoveries ranged from 76.5% to 90.3% with relative standard deviations between 3.3% and 6.5% (n=6). The linear range was found to be 0.025-2.5 mg/L, with r2 greater than 0.99 and limit of detection of 0.007 mg/L. This method provided excellent linearity, precision, and recovery, and thus, can be applied to the analysis of diclazepam in urine due to its simplicity, accuracy, and practicality.

Key words: diclazepam, gas chromatography-mass spectrometry, liquid-liquid microextraction, switchable hydrophilicity solvent, urine

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