中空纤维膜液相微萃取-气相色谱/质谱法检测尿液中的苯丙胺类兴奋剂  

Determination of amphetamines in urine by hollow fiber-based liquid-phase microextraction and chromatography-mass spectrometry

作　　者：张文文[1] 孟品佳[1] 孟梁[1] 王丹[1] 

机构地区：[1]中国人民公安大学刑事科学技术系,北京100038

出　　处：《分析试验室》2013年第1期44-47,共4页Chinese Journal of Analysis Laboratory

基　　金：公安部应用创新计划(2011YYCXGADX128);北京教育委员会共建项目计划(SYS1004100436);中央高校基本科研业务费专项资金资助

摘　　要：建立了尿液中痕量苯丙胺类毒品的中空纤维膜液相微萃取-气相色谱/质谱检测方法。采用中空纤维膜液相微萃取技术萃取尿液中4种苯丙胺类毒品,研究萃取剂类型、体积、溶液pH、萃取时间和温度等对萃取效果的影响。尿液中4种苯丙胺类毒品的最佳萃取条件为:样品溶液pH 13,甲苯为萃取剂,搅拌速度500 r/min,30℃条件下萃取15 min;此条件下苯丙胺(AM)、甲基苯丙胺(MAM)、3,4-亚甲二氧基苯丙胺(MDA)、3,4-亚甲二氧基甲基苯丙胺(MDMA)的检出限(S/N=3)分别为1.0,0.75,1.0,0.64 ng/mL,相对标准偏差分别为6.62%,3.98%,4.57%,2.35%,富集倍数分别为155,170,132,218倍。本方法可用于尿液中痕量苯丙胺类毒品的分析测定。Objective A novel method was developed to determine the trace amounts of amphetamine-type stimulants in urine by GC-MS coupled with hollow fiber membrane solvent microextraction.Methods Hollow fiber membrane liquid phase microextraction technology was adopted to extract amphetamines in urine after optimization of extraction conditions,such as solvent,volume,pH,stirring speed,time and temperature.Results Optimization of the extraction for amphetamines in urine was： toluene being used as extraction solvent,the target analytes in urine were extracted under pH 13 with temperature at 30 ℃,stirring speed at 500 r/min,for 15 min.Under the optimized conditions,the LODs of amphetamine,methamphetamine,MDA,MDMA were 1.0,0.75,1.0 and 0.64 ng/mL;the RSDs were 6.62%,3.98%,4.57%,2.35%;and the enrichment factors were 155,170,132,218,respectively.Conclusion The results demonstrated that the method was feasible for the determination of the trace amounts of amphetamine-type stimulants in urine.

关 键 词：法医毒物分析 中空纤维膜液相微萃取 GC-MS 苯丙胺类毒品 

分 类 号：O657.63[理学—分析化学]