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由亚胺键合共价有机框架衍生的磁性多孔碳材料用于土壤中痕量含氯除草剂的磁性固相萃取。

Magnetic porous carbon material derived from imine-linked covalent organic frameworks for magnetic solid phase extraction of trace chlorine-containing herbicides in soil.

机构信息

Guangxi Colleges and Universities Key Laboratory of Food Safety and Detection, College of Chemistry and Bioengineering, Guilin University of Technology, Guangxi 541004, China; Guilin Institute of Information Technology, Guilin, Guangxi 541004, China.

Guangxi Colleges and Universities Key Laboratory of Food Safety and Detection, College of Chemistry and Bioengineering, Guilin University of Technology, Guangxi 541004, China.

出版信息

J Chromatogr A. 2024 Jan 4;1713:464497. doi: 10.1016/j.chroma.2023.464497. Epub 2023 Nov 8.

DOI:10.1016/j.chroma.2023.464497
PMID:37976904
Abstract

Here, imine-linked covalent organic frameworks coated FeO microspheres were fabricated and employed as the self-template to prepare magnetic porous carbon material. The magnetic solid phase extraction (MSPE) performance of such magnetic covalent organic frameworks derived porous carbons (CMCOFs) were studied for the first time, and the improved MSPE performance was verified. The variations of chemical and material properties in the carbonization processes were studied, and it was found that the CMCOFs carbonated at 400°C exhibited highest adsorption efficiencies for chlorine-containing herbicides due to the formation of nitrile components at this stage. The CMCOFs retained high adsorption efficiencies (above 90 %) to chlorine-containing herbicides at wide pH range (3-12) and high salt concentration. The CMCOFs-based MSPE coupled with HPLC technique was in good potential for analysis of trace chlorine-containing herbicides in soil samples. Under the optimized conditions, this approach displayed short extraction and elution time (5 and 8 min) and low limits of detection (0.35-5.5 ng/mL) for chlorine-containing herbicides. The recoveries of spiked analytes and the relative standard deviations in real soil samples were 81.86 %-110.9 % and less than 5.92 %, respectively. This study provides an efficient method for the analysis of trace chlorine-containing herbicides in complex samples, as well as give some inspiration on material modulation by controlled carbonization to achieve improved sorption performances.

摘要

在这里,我们制备了亚胺键连接的共价有机框架包覆的 FeO 微球,并将其用作自模板来制备磁性多孔碳材料。首次研究了这种磁性共价有机框架衍生的多孔碳(CMCOFs)的磁性固相等离子体萃取(MSPE)性能,并验证了其改进的 MSPE 性能。研究了碳化过程中化学和材料性质的变化,发现 CMCOFs 在 400°C 碳化时由于在该阶段形成了腈基组分,对含氯除草剂表现出最高的吸附效率。CMCOFs 在宽 pH 范围(3-12)和高盐浓度下对含氯除草剂仍保持高吸附效率(高于 90%)。基于 CMCOFs 的 MSPE 与 HPLC 技术相结合,在分析土壤样品中的痕量含氯除草剂方面具有良好的应用潜力。在优化条件下,该方法对含氯除草剂的萃取和洗脱时间(5 和 8 分钟)较短,检测限(0.35-5.5ng/mL)较低。加标分析物在实际土壤样品中的回收率和相对标准偏差分别为 81.86%-110.9%和小于 5.92%。本研究为分析复杂样品中的痕量含氯除草剂提供了一种有效的方法,并为通过控制碳化来调节材料以实现改进的吸附性能提供了一些启示。

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