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采用微波辅助溶剂萃取和连续固相萃取-气相色谱-质谱联用技术测定环境固体样品中的13种内分泌干扰化学物

Determination of 13 endocrine disrupting chemicals in environmental solid samples using microwave-assisted solvent extraction and continuous solid-phase extraction followed by gas chromatography-mass spectrometry.

作者信息

Azzouz Abdelmonaim, Ballesteros Evaristo

机构信息

Department of Physical and Analytical Chemistry, E.P.S. of Linares, University of Jaén, 23700, Linares, Jaén, Spain.

出版信息

Anal Bioanal Chem. 2016 Jan;408(1):231-41. doi: 10.1007/s00216-015-9096-1. Epub 2015 Oct 16.

Abstract

Soil can contain large numbers of endocrine disrupting chemicals (EDCs). The varied physicochemical properties of EDCs constitute a great challenge to their determination in this type of environmental matrix. In this work, an analytical method was developed for the simultaneous determination of various classes of EDCs, including parabens, alkylphenols, phenylphenols, bisphenol A, and triclosan, in soils, sediments, and sewage sludge. The method uses microwave-assisted extraction (MAE) in combination with continuous solid-phase extraction for determination by gas chromatography-mass spectrometry. A systematic comparison of the MAE results with those of ultrasound-assisted and Soxhlet extraction showed MAE to provide the highest extraction efficiency (close to 100%) in the shortest extraction time (3 min). The proposed method provides a linear response over the range 2.0 - 5000 ng kg(-1) and features limits of detection from 0.5 to 4.5 ng kg(-1) depending on the properties of the EDC. The method was successfully applied to the determination of target compounds in agricultural soils, pond and river sediments, and sewage sludge. The sewage sludge samples were found to contain all target compounds except benzylparaben at concentration levels from 36 to 164 ng kg(-1). By contrast, the other types of samples contained fewer EDCs and at lower concentrations (5.6 - 84 ng kg(-1)).

摘要

土壤中可能含有大量内分泌干扰化学物质(EDCs)。EDCs多样的物理化学性质给在这类环境基质中对其进行测定带来了巨大挑战。在本研究中,开发了一种分析方法,用于同时测定土壤、沉积物和污水污泥中的各类EDCs,包括对羟基苯甲酸酯、烷基酚、苯基酚、双酚A和三氯生。该方法采用微波辅助萃取(MAE)结合连续固相萃取,通过气相色谱 - 质谱联用进行测定。将MAE的结果与超声辅助萃取和索氏萃取的结果进行系统比较,结果表明MAE在最短萃取时间(3分钟)内提供了最高的萃取效率(接近100%)。所提出的方法在2.0 - 5000 ng kg⁻¹范围内呈线性响应,根据EDC的性质,检测限为0.5至4.5 ng kg⁻¹。该方法成功应用于测定农业土壤、池塘和河流沉积物以及污水污泥中的目标化合物。发现污水污泥样品中除对羟基苯甲酸苄酯外含有所有目标化合物,浓度范围为36至164 ng kg⁻¹。相比之下,其他类型的样品中EDCs含量较少且浓度较低(5.6 - 84 ng kg⁻¹)。

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