Department of Forensic Science, Chinese People's Public Security University, Beijing 100038, PR China.
Forensic Sci Int. 2011 Jun 15;209(1-3):42-7. doi: 10.1016/j.forsciint.2010.12.003. Epub 2010 Dec 30.
A new method was developed for pre-concentration, chiral separation and determination of multiple illicit drugs on forensic samples using dispersive liquid-liquid microextraction (DLLME) and capillary electrophoresis (CE) with Ultra Violet (UV) detection. The method was based on the formation of tiny droplets of an organic extractant in the prepared sample solution using water-immiscible organic solvent (chloroform) dissolved in water-miscible organic dispersive solvent (isopropyl alcohol). The organic phase, which extracted heroin, DL-methamphetamine, DL-3, 4-methylenedioxymethamphetamine and dl-ketamine from the prepared sample solution, was separated by centrifuging. The sedimented phase was transferred into a small volume CE auto-sampler vial with 10 μL of 1% HCl methanol solution and evaporated to dryness. The residue was reconstituted in lidocaine hydrochloride aqueous solution (internal standard) and introduced by electrokinetic injection into CE. Parameters affecting extraction efficiency were investigated and optimized. Under optimum conditions, linearity of the method was 0.15-6500 μg/L for all target analytes. The LODs (S/N=3) were 0.05-0.20 μg/L. Excellent repeatability (RSD ≤ 4.4%, n=5) was achieved. The feasibility of this method was demonstrated by analyzing spiked forensic samples. To our knowledge, it is the first time to combine DLLME with CE for chiral separation and determining illicit drugs on forensic samples.
一种新的方法被开发出来,用于在法医样本中使用分散液-液微萃取(DLLME)和带有紫外(UV)检测的毛细管电泳(CE)对多种非法药物进行预浓缩、手性分离和定量。该方法基于在制备的样品溶液中形成微小的有机溶剂液滴,有机溶剂(氯仿)溶解在水混有机溶剂(异丙醇)中。有机相从制备的样品溶液中提取海洛因、DL-甲基苯丙胺、DL-3,4-亚甲基二氧甲基苯丙胺和 dl-氯胺酮,通过离心分离。将沉淀相转移到一个小体积的 CE 自动进样小瓶中,用 10 μL 1% HCl 甲醇溶液洗脱并蒸发至干燥。残渣在盐酸利多卡因水溶液(内标)中重新溶解,并通过电动进样引入 CE。考察并优化了影响萃取效率的参数。在最佳条件下,所有目标分析物的方法线性范围为 0.15-6500 μg/L。LODs(S/N=3)为 0.05-0.20 μg/L。获得了出色的重复性(RSD≤4.4%,n=5)。该方法的可行性通过分析加标法医样本得到了验证。据我们所知,这是首次将 DLLME 与 CE 结合用于法医样本中非法药物的手性分离和定量。