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Medium to highly polar pesticides in seawater: Analysis and fate in coastal areas of Catalonia (NE Spain)

机译：海水中至高极性农药：加泰罗尼亚沿海地区的分析和命运（西班牙东北）

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摘要

Pollution has been less investigated in marine and coastal environments than in inland waters. The low levels at which pollutants are expected to be present in seawater calls for the use of reliable and high sensitivity analytical methodologies. In this context, this work presents the optimization and validation of an analytical method to determine 26 medium to highly polar pesticides in seawater based on solid phase extraction and liquid chromatography-tandem mass spectrometry detection. The developed methodology was linear, accurate (relative recoveries within 80-120% for most analytes), repeatable (relative standard deviations 18% for most analytes), and sensitive (limits of determination 1 ng/L for 89% of the compounds). The use of isotopically labeled compounds as surrogate standards compensated for low analyte recoveries and matrix effects. The method was applied to the analysis of seawater samples collected along the Coastline of Catalonia (NE Spain). Overall, total pesticide loads were higher inside the marinas than outside. The booster biocides diuron and irgarol used in antifouling paintings and different triazine pesticides were the most abundant compounds. Irgarol was present above the maximum allowable concentration set in European regulations in 70% of the samples collected inside the marinas. A different pesticide pollution pattern, with MCPA and bentazone presenting the highest concentrations, was observed at the Ebro Delta area due to the impact of the agricultural activities carried out there. To the authors' knowledge, 4 out of the 26 target pesticides, namely, chlorfenvinphos, fenthion oxon, fenthion sulfone, and fenthion sulfoxide, have not been previously investigated in seawater. (C) 2018 Elsevier Ltd. All rights reserved.
机译：与内陆水域相比，海洋和沿海环境对污染的调查较少。预期海水中污染物的含量低，要求使用可靠且高灵敏度的分析方法。在此背景下，这项工作提出了一种基于固相萃取和液相色谱-串联质谱检测技术来确定海水中26种中等至高极性农药的分析方法的优化和验证。所开发的方法是线性的，准确的（大多数分析物的相对回收率在80-120％之内），可重复的（大多数分析物的相对标准偏差<18％）和灵敏的（89％化合物的测定限度<1 ng / L） ）。使用同位素标记的化合物作为替代标准品可补偿低的分析物回收率和基质效应。该方法被用于分析沿加泰罗尼亚（西班牙东北部）海岸线收集的海水样品。总体而言，码头内部的农药总量高于室外。防污涂料中使用的增强杀虫剂杜隆和依加洛尔以及不同的三嗪类农药是最丰富的化合物。在船坞内收集的样品中，有70％的样品中存在Irgarol，高于欧洲法规规定的最大允许浓度。由于那里农业活动的影响，在埃布罗三角洲地区观察到了不同的农药污染模式，其中MCPA和苯达松的浓度最高。据作者所知，以前尚未在海水中研究过26种目标农药中的4种，即氯芬芬磷，倍硫磷，氧化硫磷和倍硫磷。 （C）2018 Elsevier Ltd.保留所有权利。

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