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采用固相萃取结合液相色谱-高分辨率质谱法测定不同类型环境水样中的合成卡西酮。

Solid-phase extraction followed by liquid chromatography-high resolution mass spectrometry to determine synthetic cathinones in different types of environmental water samples.

作者信息

Fontanals N, Marcé R M, Borrull F

机构信息

Departament de Química Analítica i Química Orgànica, Universitat Rovira i Virgili, Campus Sescelades, Marcel·lí Domingo s/n, 43007 Tarragona, Spain.

Departament de Química Analítica i Química Orgànica, Universitat Rovira i Virgili, Campus Sescelades, Marcel·lí Domingo s/n, 43007 Tarragona, Spain.

出版信息

J Chromatogr A. 2017 Nov 17;1524:66-73. doi: 10.1016/j.chroma.2017.10.002. Epub 2017 Oct 4.

DOI:10.1016/j.chroma.2017.10.002
PMID:29031971
Abstract

Synthetic cathinones have become popular in recent years, which would explain why their determination in influent sewage samples has already been documented. In the present study a method based on solid-phase extraction followed by liquid chromatography and high resolution mass spectrometry is developed, validated and applied to determine twelve cathinones and one of their metabolites in different environmental samples including influent and effluent sewage and river water. Two cation-exchange sorbents (Oasis MCX and Oasis WCX) were compared, with better results achieved with Oasis WCX in terms of apparent recoveries (70-100%) and matrix effects (lower than -34%). The method was validated with effluent sewage samples providing suitable figures of merit, with method quantification limits ranging from 1ng/L to 5ng/L and method detection limits from 0.1ng/L to 0.5ng/L for all the compounds. Of the different cathinones studied, three, namely methylone, mephedrone metabolite and methylenedioxypyrovalerone, were quantified at concentration levels of low ng/L in each of the different samples analysed, while a number of the other cathinones were also detected in some of the samples.

摘要

合成卡西酮近年来广受欢迎,这可以解释为何已有文献记载在污水进水样本中对其进行测定。在本研究中,开发、验证了一种基于固相萃取,随后进行液相色谱和高分辨率质谱分析的方法,并将其应用于测定不同环境样本(包括污水进水和出水以及河水)中的十二种卡西酮及其一种代谢物。比较了两种阳离子交换吸附剂(Oasis MCX和Oasis WCX),结果表明Oasis WCX在表观回收率(70 - 100%)和基质效应(低于 - 34%)方面表现更佳。该方法通过污水出水样本进行验证,得到了合适的品质因数,所有化合物的方法定量限为1ng/L至5ng/L,方法检测限为0.1ng/L至0.5ng/L。在所研究的不同卡西酮中,在分析的每个不同样本中,有三种卡西酮,即甲酮、甲氧麻黄酮代谢物和亚甲基二氧吡咯戊酮,其浓度水平为低纳克/升,同时在一些样本中也检测到了其他一些卡西酮。

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