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Determination of parabens and endocrine-disrupting alkylphenols in soil by gas chromatography-mass spectrometry following matrix solid-phase dispersion or in-column microwave-assisted extraction: A comparative study

机译:固相分散或柱内微波辅助萃取-气相色谱-质谱法测定土壤中对羟基苯甲酸酯和破坏内分泌的烷基酚

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摘要

Two rapid methods were evaluated for the simultaneous extraction of seven parabens and two alkylphenols from soil based on matrix solid-phase dispersion (MSPD) and microwave-assisted extraction (MAE). Soil extracts were derivatized with N,O-bis(trimethylsilyl)trifluoroacetamide and analyzed by gas chromatography with mass spectrometry. Extraction and clean-up of samples were carried out by both methods in a single step. A glass sample holder, inside the microwave cell, was used in MAE to allow the simultaneous extraction and clean-up of samples and shorten the MAE procedure. The detection limits achieved by MSPD were lower than those obtained by MAE because the presence of matrix interferences increased with this extraction method. The extraction yields obtained by MSPD and MAE for three different types of soils were compared. Both procedures showed good recoveries and sensitivity for the determination of parabens and alkylphenols in two of the soils assayed, however, only MSPD yielded good recoveries with the other soil. Finally, MSPD was applied to the analysis of soils collected in different sites of Spain. In most of the samples analyzed, methylparaben and butylparaben were detected at levels ranging from 1.21 to 8.04 ng g ~(-1) dry weight and 0.48 to 1.02 ng g ~(-1) dry weight, respectively.
机译:评价了两种快速方法,基于基质固相分散体(MSPD)和微波辅助萃取(MAE)从土壤中同时提取7种对羟基苯甲酸酯和2种烷基酚。用N,O-双(三甲基甲硅烷基)三氟乙酰胺衍生土壤提取物,并通过气相色谱法和质谱法进行分析。通过两种方法在一个步骤中进行样品的提取和净化。微波池内部的玻璃样品架用于MAE中,以允许同时提取和清洁样品并缩短MAE程序。 MSPD获得的检出限低于MAE获得的检出限,因为这种萃取方法会增加基质干扰的存在。比较了MSPD和MAE对三种不同类型土壤的提取率。两种方法均显示出良好的回收率和灵敏性,可用于测定两种土壤中的对羟基苯甲酸酯和烷基酚,但是,只有MSPD可以与另一种土壤良好地回收。最后,将MSPD应用于西班牙不同地点收集的土壤分析。在大多数分析样品中,检测到的对羟基苯甲酸甲酯和对羟基苯甲酸丁酯的干重分别为1.21至8.04 ng g〜(-1)干重和0.48至1.02 ng g〜(-1)干重。

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