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制备一种基于咪唑鎓的聚(离子液体)功能化磁性三维氧化石墨烯,用于从茶叶样品中磁性固相萃取拟除虫菊酯。

Preparation of an imidazolium-based poly(ionic liquid) functionalized magnetic three-dimensional graphene oxide for magnetic solid phase extraction of pyrethroids from tea samples.

机构信息

School of Food Science and Engineering, State Key Laboratory of Biobased Material and Green Papermaking, Qilu University of Technology (Shandong Academy of Sciences), Jinan 250353, China.

School of Food Science and Engineering, State Key Laboratory of Biobased Material and Green Papermaking, Qilu University of Technology (Shandong Academy of Sciences), Jinan 250353, China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2024 Oct 15;1247:124321. doi: 10.1016/j.jchromb.2024.124321. Epub 2024 Sep 16.

Abstract

In this work, an imidazolium-based poly(ionic liquid) (poly(1-dodecyl-3-vinyl-imidazolium bromide) functionalized magnetic three-dimensional graphene oxide (FeO@3D-GO@poly(ImCBr)) was synthesized via a vacuum freezing-drying method and used as a magnetic solid phase extraction (MSPE) adsorbent for the efficient extraction of pyrethroid pesticides from tea samples. The prepared FeO@3D-GO@poly(ImCBr) was confirmed by scanning electron microscopy (SEM), Fourier transform infrared spectrometry (FT-IR), vibrating sample magnetometer (VSM) and X-ray photoelectron spectrogram (XPS). Due to its large specific surface area and the ability to offer multiple intermolecular interactions, including π-π stacking, hydrophobic and hydrogen bond interactions, the prepared FeO@3D-GO@poly(ImCBr) showed high extraction efficiency for pyrethroids. The experimental parameters were optimized by a combination of single-factor method and Box-Behnken design to improve the extraction efficiency. Under the optimum conditions, coupled with high performance liquid chromatography (HPLC), a sensitive analytical method was developed for the determination of pyrethroids, and the proposed method showed wide linear ranges (1.00-100 μg L) with correlation coefficients (R) ranging from 0.9980 to 0.9994, low limits of detection (0.100 μg L) and good repeatability with intra-day relative standard deviations (RSDs) in the range of 2.90-5.53 % and inter-day RSDs in the range of 1.83-7.76 %. Moreover, the developed method was successfully applied to the determination of pyrethroids in tea samples and satisfactory recoveries ranging from 82.37 % to 114.34 % were obtained. The results showed that the developed FeO@3D-GO@poly(ImCBr) was an ideal, effective and selective material for the extraction and enrichment of pyrethroids from tea samples.

摘要

在这项工作中,通过真空冷冻干燥法合成了一种基于咪唑鎓的聚(离子液体)(聚(1-十二烷基-3-乙烯基-咪唑溴化物)功能化磁性三维氧化石墨烯(FeO@3D-GO@poly(ImCBr)),并将其用作从茶叶样品中高效提取拟除虫菊酯农药的磁性固相萃取(MSPE)吸附剂。通过扫描电子显微镜(SEM)、傅里叶变换红外光谱(FT-IR)、振动样品磁强计(VSM)和 X 射线光电子能谱(XPS)确认了制备的 FeO@3D-GO@poly(ImCBr)。由于其具有较大的比表面积和提供多种分子间相互作用的能力,包括π-π堆积、疏水和氢键相互作用,因此制备的 FeO@3D-GO@poly(ImCBr)对拟除虫菊酯表现出高的萃取效率。通过单因素法和 Box-Behnken 设计相结合优化了实验参数,以提高萃取效率。在最佳条件下,结合高效液相色谱(HPLC),建立了一种用于测定拟除虫菊酯的灵敏分析方法,该方法具有较宽的线性范围(1.00-100μg L),相关系数(R)范围为 0.9980 至 0.9994,检测限(0.100μg L)低,日内相对标准偏差(RSD)在 2.90-5.53%范围内,日间 RSD 在 1.83-7.76%范围内,重复性好。此外,该方法成功应用于茶叶样品中拟除虫菊酯的测定,获得了 82.37%-114.34%的回收率。结果表明,开发的 FeO@3D-GO@poly(ImCBr)是一种理想、有效和选择性的从茶叶样品中提取和富集拟除虫菊酯的材料。

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