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通过简便的机械化学合成法制备磁性共价有机框架复合材料,用于高效提取湖泊水样中的微囊藻毒素。

Facile mechanochemistry synthesis of magnetic covalent organic framework composites for efficient extraction of microcystins in lake water samples.

机构信息

Ministry of Education Key Laboratory for Analytical Science of Food Safety and Biology, Fujian Provincial Key Laboratory of Analysis and Detection Technology for Food Safety, College of Chemistry, Fuzhou University, Fuzhou, Fujian, 350002, China.

Division of Chemical and Biological Engineering, Minjiang Teachers College, Fuzhou, Fujian, 350108, China.

出版信息

Anal Chim Acta. 2021 Jun 29;1166:338539. doi: 10.1016/j.aca.2021.338539. Epub 2021 Apr 19.

Abstract

Easy-preparation magnetic solid-phase extraction (MSPE) adsorbents with excellent extraction performance are very indispensable for MSPE techniques. Herein, a magnetic carbon nanotube covalent organic framework composite (MCNTs@TpPa-1) was prepared simply and rapidly through mechanochemical synthesis as MSPE adsorbent for enriching microcystins (MCs). The synthesized MCNTs@TpPa-1 exhibited well water dispersibility, high affinity with MCs and large surface area, resulting in outstanding extraction performance for MCs. Subsequently, combined with high-performance liquid chromatography with tandem mass spectrometry (HPLC-MS/MS), an efficient, sensitive and convenient MSPE method was set up for the determination of trace MCs from aqueous sample, which exhibited acceptable repeatability (RSDs (relative standard deviations) ≤ 6.8%, n = 6), low limits of detection (LODs, 0.8-1.5 pg mL), reliable linearity (R ≥ 0.9991) and broad range of linearity (2.0-1000 pg mL). Furthermore, the developed method was applied to lake samples and trace MCs (9.6-24.6 pg mL) were found with satisfactory recovery (85.0-106.0%). The results indicated powerfully MCNTs@TpPa-1 was of significant potential as an MSPE sorbent for detection of trace MCs in water. Moreover, considering the complexity of traditional preparation methods, novel prospects for preparing magnetic covalent organic frameworks (COFs) with excellent extraction properties were opened up.

摘要

一种简便、快速的通过机械化学合成制备的磁性碳纳米管共价有机框架复合材料(MCNTs@TpPa-1)用作 MSPE 吸附剂,用于富集微囊藻毒素(MCs)。所合成的 MCNTs@TpPa-1 具有良好的水分散性、与 MCs 的高亲和力和大的表面积,从而表现出出色的 MCs 萃取性能。随后,结合高效液相色谱-串联质谱(HPLC-MS/MS),建立了一种用于水样中痕量 MCs 测定的高效、灵敏、便捷的 MSPE 方法,该方法具有可接受的重复性(RSDs(相对标准偏差)≤6.8%,n=6)、低检测限(LODs,0.8-1.5pgmL)、可靠的线性(R≥0.9991)和较宽的线性范围(2.0-1000pgmL)。此外,该方法被应用于湖泊样品中,发现痕量 MCs(9.6-24.6pgmL)的回收率令人满意(85.0-106.0%)。结果表明,MCNTs@TpPa-1 作为一种用于水中痕量 MCs 检测的 MSPE 吸附剂具有很大的潜力。此外,考虑到传统制备方法的复杂性,为制备具有优异萃取性能的磁性共价有机框架(COFs)开辟了新的前景。

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