分散液相微萃取-毛细管电泳法同时检测唾液中的8种毒品  

Determination of Drugs of Abuse in Saliva by Dispersive Liquid-Liquid Microextraction Coupled with Capillary Zone Electrophoresis

作　　者：孟梁[1] 王燕燕[1] 孟品佳[1] 王彦吉[1] 张强 

机构地区：[1]中国人民公安大学刑事科学技术系,北京100038 [2]内蒙古自治区公安厅刑侦总队,呼和浩特010051

出　　处：《分析化学》2011年第7期1077-1082,共6页Chinese Journal of Analytical Chemistry

基　　金：北京教育委员会共建项目计划(No.SYS1004100436)资助项目

摘　　要：建立了分散液相微萃取与毛细管电泳光电二极管阵列检测法检测唾液中的阿片类、苯丙胺类及氯胺酮等8种毒品的新方法。对影响萃取富集效率的因素进行优化:将0.5 mL含有41μL三氯甲烷的异丙醇混合溶液快速注入到5.0 mL样品溶液中,分散混匀后,以4000 r/min离心5 min,移取萃取溶剂并以氮气吹干;再用含有内标物的水溶液溶解后供毛细管电泳分析。在优化条件下,富集倍数达555～631倍;各药物在0.15～6000μg/L浓度范围内存在良好的线性关系,r为0.9986～0.9994;检出限为0.055～0.135μg/L(S/N=3);RSD<4.0%(n=5)。本方法成功应用于唾液中8种毒品的检测,平均加标回收率在85.6%～99.4%之间;检出限为1.5～3.0μg/L(S/N=3);RSD<5.1%(n=5)。本方法具有操作简单、富集效率高、灵敏度高和干扰小等特点,可用于生物样品中痕量毒品的检测。A novel method was developed for the pre-concentration and determination of eight drugs in saliva by dispersive liquid-liquid microextraction（DLLME） coupled with capillary zone electrophoresis with photo diode array detection（CE-PDA）.Parameters affecting extraction efficiency were investigated and optimized.In the method,0.5 mL isopropyl alcohol containing 41.0 μL chloroform was rapidly injected into a 5.0-mL saliva sample.After centrifugation at 4000 r/min for 5 min,the sedimented phase was transferred into a small volume CE auto-sampler vial and evaporated to dryness.The residue was reconstituted in lidocaine hydrochloride（internal standard） aqueous solution and introduced by electrokinetic injection into CE.Under the optimum conditions,linearity of the method was observed for all target analytes in the range from 0.15 to 6000 μg/L with the correlation coefficient（r） ranging from 0.9986 to 0.9994.The LODs（S/N=3） were estimated to be in the range from 0.055 to 0.135 μg/L.Excellent repeatability of the extraction（RSD≤4.0%,n=5） was achieved.As high as 555 to 631 fold enrichment factors were achieved.The feasibility of this method was demonstrated by determination of drugs in saliva samples with spiked recoveries in the range of 85.6～99.4%（RSD≤5.1%,n=5）.The method was proven to be simple and environmental benign with high enrichment factor and low cost.

关 键 词：分散液相微萃取 毛细管电泳 阿片类毒品 苯丙胺类毒品 氯胺酮 唾液 

分 类 号：D919.2[医药卫生—法医学]