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含羟基多孔有机骨架涂层搅拌棒吸附萃取结合高效液相色谱-二极管阵列检测器分析葡萄和甘蓝样品中的三唑类杀菌剂。

Hydroxyl-containing porous organic framework coated stir bar sorption extraction combined with high performance liquid chromatography-diode array detector for analysis of triazole fungicides in grape and cabbage samples.

机构信息

Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, China.

Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, China.

出版信息

J Chromatogr A. 2020 Dec 6;1633:461628. doi: 10.1016/j.chroma.2020.461628. Epub 2020 Oct 15.

DOI:10.1016/j.chroma.2020.461628
PMID:33128975
Abstract

In this work, a hydroxyl-containing porous organic framework (HC-POF) was prepared by a simple solvothermal reaction with 1,4-phthalaldehyde and phloroglucinol as monomers. Sol-gel method was used to coat HC-POF on the glass stir bar. The prepared HC-POF coated stir bar shows better extraction performance for six triazole fungicides (TFs) compared to commercial polydimethylsiloxane and ethylene glycol-silicone coated stir bars. Fourier transform infrared Spectrometry and X-ray photoelectron Spectrometry were used to explore interactions between HC-POF coating and TFs. It is assumed that the coating mainly adsorbs TFs through π-π interactions, hydrogen bonding and hydrophobic interactions. Based on this fact, a new method of HC-POF coated stir bar sorptive extraction combined with high performance liquid chromatography-diode array detector was developed for the determination of six TFs in grape and cabbage samples. A series of extraction and desorption conditions were carefully optimized, including salt concentration, sample solution pH, stirring rate and desorption solvent. Under the optimized experimental conditions, the proposed method displayed limits of detection in the range of 0.022 -0.071 μg L, which is the lowest among the reported SBSE methods for target TFs analysis. The linear range for six TFs was 0.1/0.2-500 μg L and the recoveries for the spiked grape and cabbage were 81.0-109% and 80.7-111%, respectively.

摘要

在这项工作中,通过简单的溶剂热反应,以 1,4-邻苯二甲醛和间苯三酚为单体,制备了含有羟基的多孔有机骨架(HC-POF)。采用溶胶-凝胶法将 HC-POF 涂覆在玻璃棒上。与商业聚二甲基硅氧烷和乙二醇-硅氧烷涂覆的玻璃棒相比,所制备的 HC-POF 涂覆玻璃棒对六种三唑类杀菌剂(TFs)具有更好的萃取性能。傅里叶变换红外光谱和 X 射线光电子能谱用于研究 HC-POF 涂层与 TFs 之间的相互作用。假设涂层主要通过π-π相互作用、氢键和疏水相互作用吸附 TFs。基于这一事实,开发了一种新的 HC-POF 涂覆玻璃棒吸附萃取结合高效液相色谱-二极管阵列检测器的方法,用于测定葡萄和白菜样品中的六种 TFs。仔细优化了一系列萃取和洗脱条件,包括盐浓度、样品溶液 pH 值、搅拌速度和洗脱溶剂。在优化的实验条件下,该方法对六种 TFs 的检测限范围为 0.022-0.071μg L,是报道的用于目标 TFs 分析的 SBSE 方法中最低的。六种 TFs 的线性范围为 0.1/0.2-500μg L,葡萄和白菜的加标回收率分别为 81.0-109%和 80.7-111%。

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