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一种同时测定废水中50种半挥发性有机污染物的分析方法的开发。

Development of an analytical method for the simultaneous determination of 50 semi-volatile organic contaminants in wastewaters.

作者信息

Mijangos Leire, Bilbao Dennis, Lopez-Herguedas Naroa, Ortueta Natalia, Olivares Maitane, Zuloaga Olatz, Etxebarria Nestor, Prieto Ailette

机构信息

Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), Leioa, Basque Country, Spain.

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

出版信息

MethodsX. 2023 Jun 11;11:102252. doi: 10.1016/j.mex.2023.102252. eCollection 2023 Dec.

Abstract

This work describes the development of a robust analytical methodology for the simultaneous determination of 50 semi-volatile organic compounds (SVOCs) in wastewater effluent samples by solid-phase extraction (SPE) followed by gas chromatography coupled to mass spectrometry (GC-MS) analysis. In this work, we studied extensively whether the validated SPE method used for the analysis of polar compounds in wastewaters could be extended to the analysis of non-polar compounds in the same analytical run. To that aim, the effect of different organic solvents in the SPE process (i.e., sample conditioning prior to SPE, elution solvent and evaporation steps) was evaluated. In this sense, the addition of methanol to wastewater samples before the extraction, the use of hexane:toluene (4:1, v/v) mixture for the quantitative elution of target compounds, and the addition of isooctane during the evaporation were required to minimize analyte losses during SPE and enhance extraction yields. Overall, the developed methodology showed a good performance for the determination of 50 SVOCs, and was further applied to the analysis of real wastewater effluent samples.•A validated SPE method for polar compounds was extended to the analysis of non-polar compounds.•Elution with hex:tol (4:1, v/v) and the addition of isooctane during the evaporation yield good recoveries.•The developed methodology was suitable for the determination of 50 SVOCs in aqueous samples.

摘要

本工作描述了一种稳健的分析方法的开发,该方法用于通过固相萃取(SPE),随后进行气相色谱-质谱联用(GC-MS)分析,同时测定废水排放样品中的50种半挥发性有机化合物(SVOCs)。在本工作中,我们广泛研究了用于分析废水中极性化合物的经过验证的SPE方法是否可以扩展到在同一分析流程中分析非极性化合物。为此,评估了SPE过程中不同有机溶剂的影响(即SPE之前的样品预处理、洗脱溶剂和蒸发步骤)。从这个意义上讲,在萃取前向废水样品中添加甲醇、使用己烷:甲苯(4:1,v/v)混合物对目标化合物进行定量洗脱以及在蒸发过程中添加异辛烷,对于最大限度减少SPE过程中的分析物损失和提高萃取产率是必要的。总体而言,所开发的方法在测定50种SVOCs方面表现良好,并进一步应用于实际废水排放样品的分析。

•用于极性化合物的经过验证的SPE方法扩展到了非极性化合物的分析。

•用己烷:甲苯(4:1,v/v)洗脱以及在蒸发过程中添加异辛烷可实现良好的回收率。

•所开发的方法适用于测定水性样品中的50种SVOCs。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/6079/10277571/32bce7c993ee/ga1.jpg

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