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用电增强单滴微萃取-衍生化结合气相色谱法测定人尿中的苯丙胺和甲基苯丙胺。

Efficient determination of amphetamine and methylamphetamine in human urine using electro-enhanced single-drop microextraction with in-drop derivatization and gas chromatography.

机构信息

School of Public Security & Technology, Gansu Institute of Political Science and Law, Lanzhou, 730070, PR China.

School of Public Security & Technology, Gansu Institute of Political Science and Law, Lanzhou, 730070, PR China.

出版信息

Anal Chim Acta. 2019 Jan 3;1045:162-168. doi: 10.1016/j.aca.2018.09.024. Epub 2018 Sep 15.

Abstract

An efficient method for the determination of amphetamine (AM) and methylamphetamine (MA) using electro-enhanced single-drop microextraction (EE-SDME) and gas chromatography has been developed. One advantage of this method is that the extraction efficiency is greatly enhanced by the electric field acceleration of the mass transfer of target analytes from the sample solution to the organic solvent drop. In addition, the extracted analytes were in situ derivatized with isobutyl chloroformate (IBCF) in the droplet, which further improved the sensitivity of this method. Under the optimum conditions, the enrichment factors (EFs) for AM and MA were 247 and 782, respectively. The proposed method exhibited low limits of detection (0.27 μg/L for AM and 0.14 μg/L for MA) and good linearity over the concentration range between 1 and 2000 μg/L with regression coefficients (r) of more than 0.99. The intra- and interday recoveries were from 89.6 to 96.2% and 82.7-90.5%, respectively, and the intra- and interday precisions (RSDs) were from 5.2 to 8.3% and 8.9-12.8%. The proposed method was applied to the determination of amphetamines in a urine sample.

摘要

本文建立了一种使用电增强单滴微萃取(EE-SDME)和气相色谱法测定苯丙胺(AM)和甲基苯丙胺(MA)的高效方法。该方法的一个优点是,通过电场加速目标分析物从样品溶液向有机溶剂滴的质量转移,大大提高了萃取效率。此外,在液滴中用异丁基氯甲酸酯(IBCF)原位衍生化,进一步提高了该方法的灵敏度。在最佳条件下,AM 和 MA 的富集因子(EF)分别为 247 和 782。该方法的检出限低(AM 为 0.27μg/L,MA 为 0.14μg/L),在 1-2000μg/L 浓度范围内具有良好的线性关系,相关系数(r)均大于 0.99。日内和日间回收率分别为 89.6-96.2%和 82.7-90.5%,日内和日间精密度(RSD)分别为 5.2-8.3%和 8.9-12.8%。该方法应用于尿液样品中苯丙胺的测定。

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