Meng Liang, Ye Shuhai, Wu Yilin, You Linda
Department of Forensic Science, Fujian Police College, Fuzhou, China.
Institute of Forensic Science, Fujian Provincial Public Security Department, Fuzhou, China.
Forensic Sci Res. 2021 Dec 9;7(2):265-271. doi: 10.1080/20961790.2021.1986771. eCollection 2022.
A new method was developed for pre-concentration and determination of multiple drugs of abuse in human urine using dispersive liquid-liquid microextraction (DLLME) and capillary electrophoresis (CE) with photodiode array 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 eight drugs of abuse from the prepared urine solution, was separated by centrifugation. 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 (internal standard) aqueous solution and introduced by electrokinetic injection into CE. Under the optimum conditions, acceptable linear relationship was observed in the range of 3.0-500 ng/mL with the correlation coefficient () of 0.9982-0.9994 for spiked urine samples. The limit of detection (LOD) (S/N = 3) was estimated to be 1.0 ng/mL. A recovery of 75.7%-90.6% was obtained for spiked samples. The mean relative error (MRE) was within ±7.0% and the relative standard deviation (RSD) was less than 6.9%. The proposed DLLME-CE procedure offers an alternative analytical approach for the sensitive detection of drugs of abuse in real urine samples.Key pointsThe dispersive liquid-liquid microextraction (DLLME) was involved for the determination of drugs in urine with capillary electrophoresis with photodiode array detection (CE-PDA).Good linearity, sensitivity, recovery and precision were achieved.The proposed method was eco-friendly with microliter scale solvent consumption.
开发了一种新方法，用于使用分散液液微萃取（DLLME）和具有光电二极管阵列检测的毛细管电泳（CE）对人尿液中的多种滥用药物进行预浓缩和测定。该方法基于使用溶解在与水混溶的有机分散溶剂（异丙醇）中的与水不混溶的有机溶剂（氯仿）在制备的样品溶液中形成有机萃取剂的微小液滴。从制备的尿液溶液中萃取八种滥用药物的有机相通过离心分离。将沉淀相转移到含有10 μL 1%盐酸甲醇溶液的小体积CE自动进样瓶中并蒸发至干。残余物用盐酸利多卡因（内标）水溶液复溶，并通过电动进样引入CE。在最佳条件下，加标尿液样品在3.0 - 500 ng/mL范围内观察到可接受的线性关系，相关系数（）为0.9982 - 0.9994。检测限（LOD）（S/N = 3）估计为1.0 ng/mL。加标样品的回收率为75.7% - 90.6%。平均相对误差（MRE）在±7.0%以内，相对标准偏差（RSD）小于6.9%。所提出的DLLME - CE程序为实际尿液样品中滥用药物的灵敏检测提供了一种替代分析方法。关键点分散液液微萃取（DLLME）用于通过具有光电二极管阵列检测的毛细管电泳（CE - PDA）测定尿液中的药物。实现了良好的线性、灵敏度、回收率和精密度。所提出的方法具有环保性，溶剂消耗为微升级。
