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采用聚醚砜微萃取结合液相色谱-串联质谱法同时测定环境水样中的41种多类有机污染物。

Simultaneous determination of 41 multiclass organic pollutants in environmental waters by means of polyethersulfone microextraction followed by liquid chromatography-tandem mass spectrometry.

作者信息

Mijangos Leire, Ziarrusta Haizea, Olivares Maitane, Zuloaga Olatz, Möder Monika, Etxebarria Nestor, Prieto Ailette

机构信息

Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), P.O. Box 644, 48080, Bilbao, Spain.

Research Centre for Experimental Marine Biology and Biotechnology (PIE), University of the Basque Country (UPV/EHU), Areatza z/g, 48620, Plentzia, Spain.

出版信息

Anal Bioanal Chem. 2018 Jan;410(2):615-632. doi: 10.1007/s00216-017-0763-2. Epub 2017 Dec 6.

Abstract

A new procedure using polyethersulfone (PES) microextraction followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis was developed in this work for the simultaneous determination of 41 multiclass priority and emerging organic pollutants including herbicides, hormones, personal care products, and pharmaceuticals, among others, in seawater, wastewater treatment plant (WWTP) effluents, and estuary samples. The optimization of the analysis included two different chromatographic columns and different variables (polarity, fragmentor voltage, collision energy, and collision cell accelerator) of the mass spectrometer. In the case of PES extraction, ion strength of the water, pH, addition of EDTA, and the amount of the polymeric material were thoroughly investigated. The developed procedure was compared with a previously validated one based on a standard solid-phase extraction (SPE). In contrast to the SPE protocol, the PES method allowed a cost-efficient extraction of complex aqueous samples with lower matrix effect from 120 mL of water sample. Satisfactory and comparable apparent recovery values (80-119 and 70-131%) and method quantification limits (MQLs, 0.4-26 and 0.2-23 ng/L) were obtained for PES and SPE procedures, respectively, regardless of the matrix. Repeatability values lower than 27% were obtained. Finally, the developed methods were applied to the analysis of real samples from the Basque Country and irbesartan, valsartan, acesulfame, and sucralose were the analytes most often detected at the highest concentrations (51-1096 ng/L). Graphical abstract Forty-one multiclass pollutant determination in environmental waters by means of PES/SPE-LC-MS/MS.

摘要

本研究开发了一种新方法,该方法采用聚醚砜(PES)微萃取,随后进行液相色谱 - 串联质谱(LC-MS/MS)分析,用于同时测定海水中、污水处理厂(WWTP)出水和河口样品中的41种多类优先控制和新兴有机污染物,包括除草剂、激素、个人护理产品和药品等。分析的优化包括两种不同的色谱柱以及质谱仪的不同变量(极性、碎裂电压、碰撞能量和碰撞池加速器)。在PES萃取的情况下,对水的离子强度、pH值、EDTA的添加量以及聚合物材料的用量进行了深入研究。将所开发的方法与先前基于标准固相萃取(SPE)验证的方法进行了比较。与SPE方案相比,PES方法能够从120 mL水样中以较低的基质效应经济高效地萃取复杂的水性样品。无论基质如何,PES和SPE方法分别获得了令人满意且可比的表观回收率值(80 - 119%和70 - 131%)以及方法定量限(MQLs分别为0.4 - 26 ng/L和0.2 - 23 ng/L)。获得了低于27%的重复性值。最后,将所开发的方法应用于巴斯克地区实际样品的分析,厄贝沙坦、缬沙坦、乙酰磺胺酸钾和三氯蔗糖是最常检测到的高浓度分析物(51 - 1096 ng/L)。图形摘要 通过PES/SPE-LC-MS/MS测定环境水中的41种多类污染物

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