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[利用微波萃取-气相色谱法同时测定人血液中可卡因及其代谢物芽子碱甲酯]

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

作者信息

Wang Xiaobo, Ye Nengsheng, Wang Jifen, Gu Xuexin

机构信息

Department of Chemistry, Capital Normal University, Beijing 100048, China.

出版信息

Se Pu. 2010 Jul;28(7):673-6. doi: 10.3724/sp.j.1123.2010.00673.

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 degrees C 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.

摘要

建立了一种使用气相色谱 - 质谱联用仪(GC - MS)和气相色谱 - 火焰离子化检测器(GC - FID)同时测定人血液中可卡因(COC)及其代谢产物芽子碱甲酯(EME)的方法。血样采用微波萃取(MWE)进行制备。MWE的最佳参数如下:6 mL氯仿 - 异丙醇(9:1,v/v)混合液作为萃取溶剂,用0.05 mol/L Na2CO3 - NaHCO3缓冲液将样品pH值调至10.0,在40℃下萃取6分钟。萃取液中的COC和EME用GC - MS进行定性,用GC - FID进行定量。COC和EME的平均回收率为79.91%至99.85%,相对标准偏差小于3.10%,检测限(LOD)分别为60和40 mg/L。该方法无需衍生化即可检测COC和EME。该方法快速、准确、灵敏,可用于同时测定血样中的COC和EME。

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