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微波萃取-气相色谱法测定尿液中的苯丙胺类毒品

Determination of amphetamines in human urine using microwave extraction-gas chromatography

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【作者】 王继芬孙洪峰叶能胜谷学新李文君李瑛

【Author】 WANG Jifen1,SUN Hongfeng2,YE Nengsheng2,GU Xuexin2,LI Wenjun1,LI Ying1(1.Department of Criminal Science and Technology,Chinese People’s Public Security University,Beijing 100038,China;2.Department of Chemistry,Capital Normal University,Beijing 100037,China)

【机构】 中国人民公安大学刑事科学技术系首都师范大学化学系中国人民公安大学刑事科学技术系 北京100038北京100037北京100038

【摘要】 建立了人体尿液中甲基苯丙胺(MA)、3,4-亚甲二氧基苯丙胺(MDA)、3,4-亚甲二氧基甲基苯丙胺(MDMA)的微波萃取-气相色谱(GC)测定方法。分别考察了萃取溶剂种类、用量、pH值以及萃取温度、时间等因素对萃取率的影响。实验结果表明,尿液中MA,MDA,MDMA的最佳提取条件为:调节尿样pH为12,以环己烷为萃取溶剂,于40℃下微波提取10min。在此条件下MA,MDA,MDMA的平均回收率分别为92.25%,85.94%和91.50%,相对标准偏差分别为5.5%,5.5%和6.1%(n=5),提取液经气相色谱-氢火焰离子化检测器(GC-FID)检测,3种药物与基体得到了很好的分离,对尿液中MA,MDA,MDMA的最低检测限分别为10,20和20ng/mL。该方法未对药物进行衍生化,是一种快速、准确、灵敏度高的同时测定尿液中MA,MDA,MDMA的方法。

【Abstract】 A method has been developed for the determination of methamphetamine(MA),3,4-methylenedioxyamphetamine(MDA)and 3,4-methylenedioxymethamphetamine(MDMA)in human urine using microwave extraction-gas chromatography(GC).To improve the extraction efficiency,experimental parameters of the extraction,including extraction solvent and its amount,pH value of the urine sample,extraction time and temperature were investigated.The optimal conditions were as follows:the pH value of urine sample at pH 12,cyclohexane as extraction solvent,extraction at 40 ℃ for 10 min.The average recoveries of MA,MDA and MDMA with this extraction method were 92.25%,85.94% and 91.50%,the relative standard deviations were 5.5%,5.5% and 6.1%(n=5),and the limits of detection were 10,20 and 20 ng/mL,respectively.Using this method,MA,MDA and MDMA need not be derivatized and can be separated from the matrix.The results indicate that the developed method is rapid,accurate and sensitive,and can be used for the simultaneous determination of MA,MDA and MDMA in urine samples.

【基金】 中国人民公安大学院士基金项目(No.LG027-6);北京市教育委员会共建项目建设计划资助(编号JD100410669)
  • 【文献出处】 色谱 ,Chinese Journal of Chromatography , 编辑部邮箱 ,2008年02期
  • 【分类号】D919.2
  • 【被引频次】20
  • 【下载频次】520
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