生物样品中苯丙胺类毒品的小体积液相萃取及GC/MS分析  

Small-volume Liquid Extraction of Amphetamines from Bio-samples and GC/MS Analysis

作　　者：孟品佳[1] 王燕燕[1] 朱丹[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：《应用化学》2008年第12期1448-1454,共7页Chinese Journal of Applied Chemistry

基　　金：北京教育委员会共建项目建设计划(SYS1004100436)

摘　　要：考察了生物检材中4种苯丙胺类毒品,即苯丙胺(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)的液相小体积萃取方法的影响因素;考察了常规体积液相萃取与小体积液相萃取效率,考察了小体积萃取溶剂、萃取体积、待测物浓度对萃取效率的影响;对小体积萃取机制进行了初步的探讨。结果表明,在小体积萃取中,由于有机相液膜的比例大,萃取过程以液膜的吸附作用为主。当水相中待测物浓度很低时,这一萃取方式有明显的富集效果。用这一萃取方式对唾液、毛发中的该类毒品进行了提取,并直接抽取有机相进行GC分析或衍生化后GC分析。当采用GC/MS中SIM方式检测时,唾液中的最低检测限为5×10-8g/mL。毛发中的毒品经过MBTFA三氟乙酰化后,最小检测限为5×10-11g/mg毛发。实验数据证明,此提取方法得到的各项定量参数均符合分析要求。方法简便、灵敏、经济、快速,适用于生物检材中该类毒品的分析。The presented study is focused on the investigation of influence factors and mechanism of smallvolume liquid extraction of four amphetamines, named amphetamine （AM）, methamphetamine （MAM）, 3,4- methylenedioxyamphetamine（MDA） and 3,4-methylenemethamphtamine（MDMA） in biological samples. The extraction efficiencies between regular volume and small volume extraction methods were compared; some influence factors for small-volume liquid extraction such as the type and volume of organic solvent, concentration of target analytes in aqueous phase were examined, and the mechanism was studied preliminarily. It was shown that small-volume liquid extraction has a certain effect on the enrichment of analytes, the smaller the volume was, and also the lower the analytes concentration in aqueous solution was, the greater the enrichment gained. It could be deduced that organic film between organic and aqueous phases played an important role in the enrichment. Some biological specimens such as saliva and hair were extracted by means of the method. The organic phase was directly injected into GC for analysis, or transferred into another vial for derivatization after extraction. The LOD for these amphetamines was 5 × 10^-8 g/mL in saliva with GC/MS-SIM without deri- vatization, and 5 × 10^-11 g/mg in hair after MBTFA derivatization. The method validation data demonstrate that all parameters such as linearity, repeatability, relative standard variation and accuracy can meet the requirement for the drug analysis. The extraction procedure is simple, sensitive, economic and time-saving, and can be used for the analysis of the drugs in biological specimens.

关 键 词：小体积液相萃取 苯丙胺毒品 唾液 毛发 GC/MS 

分 类 号：O652[理学—分析化学]