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基于 MIL-101 吸附剂的固相萃取-气相色谱串联质谱法分析水中多类有机紫外滤光剂。

Solid-phase extraction based on MIL-101 adsorbent followed by gas chromatography tandem mass spectrometry for the analysis of multiclass organic UV filters in water.

机构信息

Center of Excellence for Innovation in Chemistry, Department of Chemistry, Faculty of Science, Prince of Songkla University, Hat Yai, Songkhla 90112, Thailand; Laboratory of Research and Development of Analytical Solutions (LIDSA), Department of Analytical Chemistry, Nutrition and Food Science, Faculty of Chemistry, Campus Vida, Universidade de Santiago de Compostela, E-15782, Santiago de Compostela, Spain.

Laboratory of Research and Development of Analytical Solutions (LIDSA), Department of Analytical Chemistry, Nutrition and Food Science, Faculty of Chemistry, Campus Vida, Universidade de Santiago de Compostela, E-15782, Santiago de Compostela, Spain.

出版信息

J Chromatogr A. 2020 Jan 11;1610:460564. doi: 10.1016/j.chroma.2019.460564. Epub 2019 Sep 22.

Abstract

A metal organic framework material MIL-101 was developed as an effective solid-phase extraction adsorbent for the extraction of eleven UV filters compounds. The MIL-101 adsorbent was packed into a polypropylene cartridge and connected at the outlet tip with the Visiprep™ vacuum manifolds allowing process up to 12-port SPE samples, simultaneously. The extracted UV filters were quantified by gas chromatography-tandem mass spectrometry. Several parameters affecting the extraction efficiency of the target analytes, i.e. desorption conditions, sample pH, the addition of salt and sample volume were optimized by ANOVA analysis followed by a multifactorial design. The sample breakthrough volume of the developed method was also evaluated. The SPE-GC-MS/MS method was validated in terms of linearity (R ≥ 0.9973), accuracy (with satisfactory recovery from 82% to 105%), precision (relative standard deviation of less than 10%) and limits of detection ranging from 1.0 to 11.7 ng L. The validated method was successfully applied for the extraction and quantification of the target UV filters in different types of water samples, including lake, river, seawater and swimming pool waters. The most often found UV filters were octocrylene, 4-methylbencylidene camphor and homosalate that also came out with the highest concentrations, up to 4000 ng L, particularly in swimming pool waters.

摘要

一种名为 MIL-101 的金属有机骨架材料被开发为一种有效的固相萃取吸附剂,用于萃取 11 种紫外线过滤化合物。MIL-101 吸附剂被填充到聚丙烯小柱中,并在出口尖端与 Visiprep™ 真空歧管连接,允许同时处理多达 12 个端口的 SPE 样品。通过气相色谱-串联质谱法对提取的紫外线过滤器进行定量分析。通过方差分析(ANOVA)和多因素设计对影响目标分析物萃取效率的几个参数(例如解吸条件、样品 pH 值、加盐量和样品体积)进行了优化。还评估了所开发方法的样品穿透体积。SPE-GC-MS/MS 方法在线性度(R≥0.9973)、准确度(回收率从 82%到 105%)、精密度(相对标准偏差小于 10%)和检测限(1.0 至 11.7ng/L)方面进行了验证。该方法成功应用于不同类型水样中目标紫外线过滤器的提取和定量分析,包括湖泊、河流、海水和游泳池水。最常发现的紫外线过滤器是奥克立林、4-甲基苄叉基樟脑和水杨酸辛酯,它们的浓度也最高,高达 4000ng/L,特别是在游泳池水中。

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