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基于具有酰胺位点的共价有机骨架的蔬菜中氨基甲酸酯类农药的高效提取与测定。

Efficient Extraction and Determination of Carbamate Pesticides in Vegetables Based on a Covalent Organic Frameworks with Acylamide Sites.

机构信息

College of Chemistry, Tianjin Key Laboratory of Biosensing and Molecular Recognition, Nankai University, Tianjin 300071, China.

College of Chemistry, Tianjin Key Laboratory of Biosensing and Molecular Recognition, Nankai University, Tianjin 300071, China; National Demonstration Center for Experimental Chemistry Education (Nankai University), Tianjin 300071, China.

出版信息

J Chromatogr A. 2022 Feb 8;1664:462799. doi: 10.1016/j.chroma.2021.462799. Epub 2022 Jan 2.

Abstract

It is an important challenge to effectively extract and determine pesticides in complex samples. Covalent organic frameworks (COFs) are burgeoning porous crystalline organic materials with good environmental resistance, thus demonstrating great potential as adsorbents in contaminants detection. In this work, we design and synthesize a novel COF-TpDB via 1,3,5-triformylphloroglucinol (Tp) and 4,4'-diaminobenzoylanilide (DB) as well as its packed cartridge for solid phase extraction (SPE) of carbamate pesticides. Simulation calculations showed H-bonding facilitates the adsorption interactions between the carbamate pesticides and TpDB. A method was developed by coupling TpDB as SPE sorbents with high performance liquid chromatography-ultraviolet (HPLC-UV) detection to determine trace carbamate pesticides in vegetables. The established method showed a wide linear range of 0.1-200 ng mL and low limit of detections (0.005-0.05 ng mL) for four carbamate pesticides. The applicability of TpDB as adsorbent was investigated for determination of trace carbamate pesticides residue in vegetables with satisfactory recoveries of four carbamates in the range of 80.4-101.2%. The results demonstrated that the COF-TpDB offer great potential for efficient extraction of carbamate pesticides from complicate matrices.

摘要

有效提取和测定复杂样品中的农药是一个重要的挑战。共价有机框架(COFs)是新兴的多孔结晶有机材料,具有良好的环境稳定性,因此在污染物检测中作为吸附剂具有很大的潜力。在这项工作中,我们通过 1,3,5-均三甲醛基苯(Tp)和 4,4'-二氨基苯甲酰苯胺(DB)设计并合成了一种新型 COF-TpDB,并将其作为固相萃取(SPE)的填充柱用于氨基甲酸酯农药的萃取。模拟计算表明氢键有利于氨基甲酸酯农药与 TpDB 之间的吸附相互作用。建立了一种将 TpDB 作为 SPE 吸附剂与高效液相色谱-紫外(HPLC-UV)检测相结合的方法,用于测定蔬菜中的痕量氨基甲酸酯农药。该方法对四种氨基甲酸酯农药的线性范围为 0.1-200ngmL,检测限(LOD)为 0.005-0.05ngmL。研究了 TpDB 作为吸附剂用于测定蔬菜中痕量氨基甲酸酯农药残留的适用性,四种氨基甲酸酯的回收率在 80.4-101.2%范围内。结果表明,COF-TpDB 为从复杂基质中高效提取氨基甲酸酯农药提供了巨大潜力。

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