色谱

色谱

• 研究论文 • 上一篇    下一篇

微波萃取-气相色谱法测定血液中的可卡因及其代谢物爱冈宁甲基酯

王小波1, 叶能胜1, 王继芬2, 谷学新1*   

  1. 1. 首都师范大学化学系, 北京 100048; 2. 中国人民公安大学刑事科学技术系, 北京 100038
  • 收稿日期:2010-01-23 修回日期:2010-03-23 出版日期:2010-07-28 发布日期:1980-03-25
  • 通讯作者: 谷学新

Simultaneous determination of cocaine and its metabolite ecgonine methyl ester in human blood using microwave extraction-gas chromatography

WANG Xiaobo1, YE Nengsheng1, WANG Jifen2, GU Xuexin1*   

  1. 1. Department of Chemistry, Capital Normal University, Beijing 100048, China; 2. Department of Criminal Science and Technology, Chinese People’s Public Security University, Beijing 100038, China
  • Received:2010-01-23 Revised:2010-03-23 Online:2010-07-28 Published:1980-03-25
  • Contact: GU Xuexin

PDF

539

被引次数

15

摘要： 建立了血液中可卡因(cocaine, COC)及其代谢物爱冈宁甲基酯(ecgonine methyl ester, EME)的气相色谱-质谱(CG-MS)和气相色谱-氢火焰离子化检测(GC-FID)方法。该方法采用微波萃取提取血液中的COC和EME,优化并确定了最佳提取条件: 以氯仿-异丙醇(体积比为9:1)混合溶液为提取溶剂,用0.05 mol/L Na2CO3-NaHCO3缓冲溶液调节样品溶液的pH至10.0,在40 ℃下微波萃取6 min；采用GC-MS对萃取液中的COC和EME进行定性,采用GC-FID进行定量检测。COC和EME的平均回收率分别为79.91%～99.85%,相对标准偏差(RSD)均小于3.10%,检出限(S/N=3)分别为60 mg/L和40 mg/L。该方法无需衍生化,快速、准确、灵敏,可同时检测血液中的COC和EME。

关键词: 爱冈宁甲基酯, 可卡因, 气相色谱-火焰离子化检测, 气相色谱-质谱, 微波萃取, 血液

Abstract: A method was developed for the simultaneous determination of cocaine (COC) and its metabolite ecgonine methyl ester (EME) in human blood using gas chromatography-mass spectrometry (GC-MS) and gas chromatography-flame ionization detection (GC-FID). The blood sample was prepared by microwave extraction (MWE). The optimal parameters of MWE were as follows: 6 mL of chloroform-isopropanol (9:1, v/v) mixture as extraction solvent, the pH value of the sample was adjusted at 10.0 with 0.05 mol/L Na2CO3-NaHCO3 buffer, the extraction was performed at 40 ℃ for 6 min. The COC and EME in the extract were qualified using GC-MS and quantitated using GC-FID. The average recoveries of COC and EME were from 79.91% to 99.85%, the relative standard deviations were less than 3.10%, and the limits of detection (LOD) were 60 and 40 mg/L, respectively. In the method COC and EME were detected without derivatization. The method is rapid, accurate and sensitive, and can be used for the simultaneous determination of COC and EME in blood samples.

Key words: cocaine, ecgonine methyl ester, gas chromatography-flame ionization detection (GC-FID), gas chromatography-mass spectrometry （GC-MS）, human blood , microwave extraction