磁性共价有机骨架固相萃取-高效液相色谱测定柑橘中农药残留

引用本文: 黄斯敏, 胡玉斐, 陈彦龙, 李攻科, 夏凌. 磁性共价有机骨架固相萃取-高效液相色谱测定柑橘中农药残留[J]. 分析化学, 2020, 48(10): 1392-1399. doi: 10.19756/j.issn.0253-3820.201359 shu

Citation: HUANG Si-Min, HU Yu-Fei, CHEN Yan-Long, LI Gong-Ke, XIA Ling. Magnetic Solid-phase Extraction Coupled with High-Performance Liquid Chromatography for Pesticide Residues Analysis in Citrus Sample[J]. Chinese Journal of Analytical Chemistry, 2020, 48(10): 1392-1399. doi: 10.19756/j.issn.0253-3820.201359 shu

磁性共价有机骨架固相萃取-高效液相色谱测定柑橘中农药残留

中山大学化学学院, 广州 510275
基金项目:
本文系广东省重点领域研发计划项目（No.2019B020211001）、国家自然科学基金项目（Nos.21675178，21976213，21804147）、国家重点研发计划项目（No.2019YFC1606101）和广东省自然科学基金项目（No.2018A030313241）资助

摘要: 制备了具有核壳结构的磁性共价有机骨架复合材料（Fe₃O₄@COF），并将其作为磁性固相萃取的吸附剂，结合高效液相色谱-紫外检测器法（HPLC-UV），建立了测定柑橘类水果中噻虫嗪、吡虫啉、多菌灵和噻菌灵等农药残留的分析方法。通过扫描电子显微镜、透射电子显微镜、傅里叶变换红外光谱、X射线粉末衍射和磁学性能测试对材料进行了表征。考察了磁性固相萃取的影响因素，得到最佳的萃取条件：将20.0 mg Fe₃O₄@COF分散于10 mL柑橘类水果样品溶液中，振荡20 min，磁性分离，用1 mL甲醇振荡5 min后洗脱，洗脱液待HPLC-UV分析。噻虫嗪、多菌灵和噻菌灵在1~1000 μg/L浓度范围内、吡虫啉在5-1000 μg/L浓度范围内与色谱峰面积具有良好的线性关系，检出限为0.27~1.22 μg/L，加标回收率为92.1%~104.0%，RSD为1.2%~8.3%。本方法操作简单，检出限低，线性范围宽，适用于柑橘类样品中的4种农药残留的同时分析。

关键词:

English

Magnetic Solid-phase Extraction Coupled with High-Performance Liquid Chromatography for Pesticide Residues Analysis in Citrus Sample

School of Chemistry, Sun Yat-sen University, Guangzhou 510275, China
Received Date: 19 June 2020
Revised Date: 04 August 2020
Fund Project:
This work was supported by the Research and Development Plan for Key Areas of Food Safety in Guangdong Province of China (No. 2019B020211001), the National Natural Science Foundation of China (Nos. 21675178, 21976213, 21804147), the National Key Research and Development Program of China (No. 2019YFC1606101) and the Guangdong Provincial Natural Science Foundation of China (No.2018A030313241).

Abstract: The Fe₃O₄@COF with core-shell structures was synthesized and used as sorbent in magnetic solid-phase extraction (MSPE). This Fe₃O₄@COF-MSPE method coupled with high-performance liquid chromatography-ultraviolet detector (HPLC-UV) was employed for simultaneous analysis of thiamethoxam, imidacloprid, carbendazim and thiabendazole residues in citrus samples. The synthesized Fe₃O₄@COF was characterized by scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectra, X-ray diffraction and magnetometry techniques. The operation conditions of MSPE were optimized. In each trial, 20.0 mg of Fe₃O₄@COF was dispersed into 10 mL of citrus sample and shaken for 20 min. Then, the Fe₃O₄@COF was separated by an external magnetic field. Next, the pesticide target compounds were eluted from Fe₃O₄@COF with 1 mL of methanol and shaken for 5 min. Under the optimized conditions, the method had an excellent linearity in the concentration range of 1-1000 μg/L for thiomethoxam, carbendazim and thiabendazle, and 5-1000 μg/L for imidacloprid. The limits of detection ranged from 0.27 μg/L to 1.22 μg/L. The recoveries ranged from 92.1% to 104.0%. The relative standard deviations (RSDs) ranged from 1.2% to 8.3%. The proposed Fe₃O₄@COF-MSPE-HPLC-UV method was demonstrated to be easy operation, low limit of detection and wide detection range, which was applicable to simultaneous determination of four pesticide residues in citrus samples.

Key words:

Magnetic solid-phase extraction
/ High performance-liquid chromatography
/ Pesticide residue
/ Citrus

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沈阳化工大学材料科学与工程学院沈阳 110142

磁性共价有机骨架固相萃取-高效液相色谱测定柑橘中农药残留

English

Magnetic Solid-phase Extraction Coupled with High-Performance Liquid Chromatography for Pesticide Residues Analysis in Citrus Sample

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

磁性共价有机骨架固相萃取-高效液相色谱测定柑橘中农药残留

English

Magnetic Solid-phase Extraction Coupled with High-Performance Liquid Chromatography for Pesticide Residues Analysis in Citrus Sample

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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