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基于分子印迹萃取的口腔液中苯丙胺类兴奋剂分析。

Amphetamine-type stimulants analysis in oral fluid based on molecularly imprinting extraction.

机构信息

Department of Analytical Chemistry, University of Valencia, 50th Dr. Moliner St., 46100, Burjassot, Spain.

Department of Analytical Chemistry, University of Valencia, 50th Dr. Moliner St., 46100, Burjassot, Spain.

出版信息

Anal Chim Acta. 2019 Apr 4;1052:73-83. doi: 10.1016/j.aca.2018.11.046. Epub 2018 Nov 24.

Abstract

A methamphetamine-based molecularly imprinted polymer (MIP) has been prepared by bulk polymerization to recognize new psychoactive substances (NPS) of the amphetamine, cathinones and 2C families in oral fluid samples, being the first precedent of a synthetized MIP for the extraction and preconcentration 32 NPS including amphetamine type substances and synthetic cathinones from oral fluids. Pre-polymerization complex and resulting materials were appropriately characterized by infrared spectroscopy, scanning electron microscopy, and nitrogen adsorption-desorption isotherms. Appropriateness of the material for the specific recognition of the target analytes was also evaluated through computational calculations and experimentally assessed by solid phase extraction (SPE). The most appropriate SPE conditions were evaluated and recoveries of 32 different NPS were obtained, ranging from 80 to 120% with a relative standard deviation (RSD) in all cases lower than 12%. Amphetamine-related NPS were analyzed by a fast and portable methodology based on ion mobility spectrometry (IMS) and a rearguard procedure based on ultra-high performance liquid chromatography coupled to mass spectrometry (UHPLC-MS) providing limit of detection values from 10 to 80 μg L and from 0.03 to 1.3 μg L, respectively. Oral fluid samples, containing different interferents like caffeine, fluticasone and cetirizine, were spiked with 300 μg L amphetamine and subsequently analyzed, showing recoveries ranging from 81 to 115% using both methodologies. Thus, this paper shows preliminary results to demonstrate the applicability of the developed procedure which could be used with minor modifications as screening technique in on-road drug analysis.

摘要

一种基于甲基苯丙胺的分子印迹聚合物(MIP)通过本体聚合制备,以识别口服液样品中的苯丙胺、卡西酮和 2C 家族的新型精神活性物质(NPS),这是首次从口服液中提取和浓缩 32 种 NPS 的合成 MIP 的先例,包括苯丙胺类物质和合成卡西酮。预聚合复合物和所得材料通过红外光谱、扫描电子显微镜和氮吸附-解吸等温线进行了适当的表征。还通过计算计算和固相萃取(SPE)实验评估了材料对目标分析物的特异性识别的适当性。评估了最合适的 SPE 条件,并获得了 32 种不同 NPS 的回收率,范围为 80-120%,所有情况下的相对标准偏差(RSD)均低于 12%。基于离子迁移谱(IMS)的快速便携方法和基于超高效液相色谱-质谱联用(UHPLC-MS)的后卫程序分析了与苯丙胺有关的 NPS,分别提供了 10-80μg/L 和 0.03-1.3μg/L 的检测限值。含有咖啡因、氟替卡松和西替利嗪等不同干扰物的口服液样品用 300μg/L 苯丙胺进行了加标,然后使用这两种方法进行了分析,回收率范围为 81-115%。因此,本文展示了初步结果,以证明所开发程序的适用性,该程序可在轻微修改后用作道路药物分析中的筛选技术。

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