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Environ Res. 2017 Jul;156:113-119. doi: 10.1016/j.envres.2017.03.023. Epub 2017 Mar 22.
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一种超临界流体色谱-串联质谱法多残留分析方法,用于分析环境样品中新兴关注的手性和非手性化学品。

A multi-residue method by supercritical fluid chromatography coupled with tandem mass spectrometry method for the analysis of chiral and non-chiral chemicals of emerging concern in environmental samples.

机构信息

Department of Chemistry, Faculty of Science, University of Bath, Bath, BA2 7AY, UK.

Material and Chemical Characterisation Facility, University of Bath, Bath, BA2 7AY, UK.

出版信息

Anal Bioanal Chem. 2020 Sep;412(23):5563-5581. doi: 10.1007/s00216-020-02780-9. Epub 2020 Jul 9.

DOI:10.1007/s00216-020-02780-9
PMID:32648103
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC7413908/
Abstract

This manuscript presents the development, validation and application of a multi-residue supercritical fluid chromatography coupled with tandem mass spectrometry method for the analysis of 140 chiral and non-chiral chemicals of emerging concern in environmental samples, with 81 compounds being fully quantitative, 14 semi-quantitative and 45 qualitative, validated according to European Medicine Agency (EMA) guidelines (European Medicines Agency 2019). One unified LC-MS method was used to analyse all analytes, which were split into three injection methods to ensure sufficient peak resolution. The unified method provided an average of 113% accuracy and 4.5% precision across the analyte range. Limits of detection were in the range of 35 pg L-0.7 μg L, in both river water and wastewater, with an average LOD of 33 ng L. The method was combined with solid-phase extraction and applied in environmental samples, showing very good accuracy and precision, as well as excellent chromatographic resolution of a range of chiral enantiomers including beta-blockers, benzodiazepines and antidepressants. The method resulted in quantification of 75% of analytes in at least two matrices, and 56% in the trio of environmental matrices of river water, effluent wastewater and influent wastewater, enabling its use in monitoring compounds of environmental concern, from their sources of origin through to their discharge into the environment.

摘要

本手稿介绍了一种多残留超临界流体色谱-串联质谱法的开发、验证和应用,用于分析环境样品中 140 种新兴关注的手性和非手性化学品,其中 81 种化合物可进行全定量分析,14 种化合物可进行半定量分析,45 种化合物可进行定性分析,验证符合欧洲药品管理局(EMA)指南(欧洲药品管理局 2019 年)。一种统一的 LC-MS 方法用于分析所有分析物,这些分析物分为三种进样方法,以确保足够的峰分辨率。统一方法在整个分析物范围内提供了平均 113%的准确度和 4.5%的精密度。在河水和废水中,检测限范围为 35 pg L-0.7 μg L,平均检测限为 33 ng L。该方法与固相萃取相结合,并应用于环境样品,显示出非常好的准确度和精密度,以及一系列手性对映异构体(包括β-受体阻滞剂、苯并二氮䓬类和抗抑郁药)的出色色谱分辨率。该方法至少在两种基质中定量了 75%的分析物,在河水、出水废水和进水废水这三种环境基质的组合中定量了 56%的分析物,使其能够用于监测环境关注化合物,从其来源到排放到环境中。