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基于金属有机骨架的磁性纳米多孔碳用于从水果样品中预浓缩有机磷农药,然后用气相色谱-火焰光度法进行检测。

Metal organic frameworks-derived magnetic nanoporous carbon for preconcentration of organophosphorus pesticides from fruit samples followed by gas chromatography-flame photometric detection.

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. 2019 Jan 4;1583:19-27. doi: 10.1016/j.chroma.2018.11.012. Epub 2018 Nov 7.

Abstract

In this work, magnetic nanoporous carbons (MNPCs) based on Zn/Co-MOFs was synthesized via a facial one-step carbonization method. The prepared MNPCs exhibited high specific surface areas, good chemical stability and high extraction efficiency for interest organophosphorus pesticides (OPPs). The good extraction performance of the MNPCs for interest OPPs can be primarily attributed to π-π interaction and hydrophobic interaction between MNPCs and OPPs. Based on it, MNPCs-based MSPE-GC-FPD method was established for the quantification of five OPPs in fruit samples. The main experimental conditions for MSPE of five target OPPs were investigated systematically and optimized, such as the desorption solvent and volume, extracted volume, ionic strength, extraction time and desorption time. Under the optimal conditions, the limits of detection (LODs, S/N = 3) were found to be in the range of 0.018 (ethion) -0.045 (malathion) μg/L. The linearity was 0.05-100 μg/L for phorate, diazinon, ethion and 0.1-100 μg/L for malathion, fenthion respectively. The reproducibility of the method was in the range of 3.5-9.7%. The recovery experiments were carried out by spiking target OPPs at three concentration levels to validate the accuracy of the proposed method, and the recoveries for target OPPs were 84-116%. The results show that the proposed method in this work can be successfully used to analyze OPPs residue in fruit sample.

摘要

在这项工作中,通过简单的一步碳化法合成了基于 Zn/Co-MOF 的磁性纳米多孔碳 (MNPCs)。所制备的 MNPCs 具有高比表面积、良好的化学稳定性和对目标有机磷农药 (OPPs) 的高萃取效率。MNPCs 对目标 OPPs 的良好萃取性能主要归因于 MNPCs 和 OPPs 之间的π-π相互作用和疏水相互作用。在此基础上,建立了基于 MNPCs 的 MSPE-GC-FPD 方法,用于测定水果样品中五种 OPPs 的含量。系统研究并优化了 MSPE 萃取五种目标 OPPs 的主要实验条件,如解吸溶剂和体积、萃取体积、离子强度、萃取时间和解吸时间。在最佳条件下,五种目标 OPP 的检出限 (LOD,S/N=3) 范围为 0.018(乙硫磷)-0.045(马拉硫磷)μg/L。线性范围为 0.05-100μg/L 用于磷胺、二嗪农、乙硫磷,0.1-100μg/L 用于马拉硫磷、硫丹分别。方法的重现性在 3.5-9.7%范围内。通过向目标 OPPs 中添加三个浓度水平的目标 OPPs 进行回收实验来验证该方法的准确性,目标 OPPs 的回收率为 84-116%。结果表明,本工作提出的方法可成功用于分析水果样品中的 OPPs 残留。

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