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一种核壳结构的磁性共价有机框架(Fe3O4@COF型),用作高效液相色谱法定量分析前对内分泌干扰酚进行固相萃取的吸附剂。

A core-shell structured magnetic covalent organic framework (type Fe3O4@COF) as a sorbent for solid-phase extraction of endocrine-disrupting phenols prior to their quantitation by HPLC.

作者信息

Deng Ze-Hui, Wang Xia, Wang Xiao-Li, Gao Cui-Ling, Dong Liang, Wang Ming-Lin, Zhao Ru-Song

机构信息

Key Laboratory for Applied Technology of Sophisticated Analytical Instruments of Shandong Province, Shandong Analysis and Test Center, Qilu University of Technology (Shandong Academy of Sciences), Jinan, 250014, China.

College of Food Science and Engineering, Shandong Agricultural University, Taian, 271018, China.

出版信息

Mikrochim Acta. 2019 Jan 14;186(2):108. doi: 10.1007/s00604-018-3198-3.

Abstract

A magnetic covalent organic framework (FeO@COF) with core-shell structure was fabricated at room temperature and used as an adsorbent for magnetic solid-phase extraction of polar endocrine-disrupting phenols (4-n-nonylphenol, 4-n-octylphenol, bisphenol A and bisphenol AF). The sorbent was characterized by transmission electron microscopy, FTIR, powder X-ray diffraction and other techniques. The main parameters governing the extraction efficiency were optimized. The phenols were quantified by HPLC with fluorometric detection. The method has attractive features such as low limits of detection (0.08-0.21 ng.mL), wide linear ranges (0.5-1000 ng.mL), and good repeatability (intra-day: 0.39%-4.99%; inter-day: 1.57%-5.21%). Satisfactory results were obtained when the developed method was applied to determine the four target pollutants in real world drink samples with spiked recoveries over the range of 81.3~118.0%. This indicates that the method is a powerful tool for the enrichment and determination of endocrine-disrupting phenols in drink samples. Graphical abstract A magnetite based covalent organic framework (FeO@COFs) was synthesized with TPAB, TPA and FeO. It was used for magnetic solid-phase extraction of endocrine-disrupting phenols from plastic-packaged tea drink samples coupled with liquid chromatography (LC) for determination.

摘要

在室温下制备了一种具有核壳结构的磁性共价有机框架(FeO@COF),并将其用作吸附剂,用于磁性固相萃取极性内分泌干扰酚类(4-正壬基酚、4-正辛基酚、双酚A和双酚AF)。通过透射电子显微镜、傅里叶变换红外光谱、粉末X射线衍射等技术对吸附剂进行了表征。对影响萃取效率的主要参数进行了优化。采用高效液相色谱荧光检测法定量分析酚类物质。该方法具有检测限低(0.08 - 0.21 ng·mL)、线性范围宽(0.5 - 1000 ng·mL)和重复性好(日内:0.39% - 4.99%;日间:1.57% - 5.21%)等优点。将所建立的方法应用于实际饮料样品中四种目标污染物的测定,加标回收率在81.3%~118.0%范围内,结果令人满意。这表明该方法是富集和测定饮料样品中内分泌干扰酚类的有力工具。图形摘要 以四丙基溴化铵、对苯二甲酸和氧化亚铁合成了基于磁铁矿的共价有机框架(FeO@COFs)。它用于从塑料包装茶饮料样品中磁性固相萃取内分泌干扰酚类,并结合液相色谱(LC)进行测定。

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