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采用磁固相萃取与毛细管区带电泳联用技术检测人尿中 8 种非法药物。

Determination of eight illegal drugs in human urine by combination of magnetic solid-phase extraction with capillary zone electrophoresis.

机构信息

Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan, PR China.

出版信息

Electrophoresis. 2011 Aug;32(16):2099-106. doi: 10.1002/elps.201100215. Epub 2011 Jul 18.

Abstract

Using magnetite/silica/poly(methacrylic acid-co-ethylene glycol dimethacrylate) (Fe(3)O(4)/SiO(2)/poly(MAA-co-EDMA)) magnetic microspheres, a rapid and high-throughput magnetic solid-phase extraction coupled with capillary zone electrophoresis (MSPE-CZE) method was developed for the determination of illegal drugs (ketamine, amphetamines, opiates, and metabolites). The MSPE of target analytes could be completed within 2 min, and the eight target analytes could be baseline separated within 15 min by CZE with 30 mM phosphate buffer solution (PBS, pH 2.0) containing 15% v/v ACN as background electrolyte. Furthermore, hydrodynamic injection with field-amplified sample stacking (FASS) was employed to enhance the sensitivity of this MSPE-CZE method. Under such optimal conditions, the limits of detection for the eight target analytes ranged from 0.015 to 0.105 μg/mL. The application feasibility of MSPE-CZE in illegal drugs monitoring was demonstrated by analyzing urine samples, and the recoveries of target drugs for the spiked sample ranging from 85.4 to 110.1%. The method reproducibility was tested by evaluating the intra- and interday precisions, and relative standard deviations of <10.3 and 12.4%, respectively, were obtained. To increase throughput of the analysis, a home-made MSPE array that has potential application to the treatment of 96 samples simultaneously was used.

摘要

使用磁铁矿/二氧化硅/聚(甲基丙烯酸-co-乙二醇二甲基丙烯酸酯)(Fe3O4/SiO2/聚(MAA-co-EDMA))磁性微球,建立了一种快速高通量的磁固相萃取结合毛细管区带电泳(MSPE-CZE)方法,用于测定非法药物(氯胺酮、苯丙胺类、阿片类药物及其代谢物)。目标分析物的 MSPE 可在 2 分钟内完成,通过 CZE 用 30 mM 磷酸盐缓冲液(PBS,pH 2.0)作为背景电解质,其中含有 15%v/v ACN,可在 15 分钟内实现 8 种目标分析物的基线分离。此外,还采用了场放大样品堆积(FASS)的动态进样来提高该 MSPE-CZE 方法的灵敏度。在这种最佳条件下,8 种目标分析物的检测限范围为 0.015 至 0.105μg/mL。通过分析尿液样本,证明了 MSPE-CZE 在非法药物监测中的应用可行性,加标样品中目标药物的回收率范围为 85.4%至 110.1%。通过评估日内和日间精密度,测试了方法的重现性,得到的相对标准偏差分别小于 10.3%和 12.4%。为了提高分析的通量,使用了一种自制的 MSPE 阵列,该阵列具有同时处理 96 个样本的潜力。

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