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  

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

作　　者：黄斯敏 胡玉斐[1] 陈彦龙 李攻科[1] 夏凌 HUANG Si-Min;HU Yu-Fei;CHEN Yan-Long;LI Gong-Ke;XIA Ling(School of Chemistry,Sun Yat-sen University,Guangzhou 510275,China)

机构地区：[1]中山大学化学学院,广州510275

出　　处：《分析化学》2020年第10期1392-1399,共8页Chinese Journal of Analytical Chemistry

基　　金：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);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1~1000μg/L浓度范围内、吡虫啉在5~1000μg/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0.27~1.22μg/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。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 1-1000μg/L for thiomethoxam,carbendazim and thiabendazle,and 5-1000μg/L for imidacloprid.The limits of detection ranged from 0.27μg/L to 1.22μg/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.

关 键 词：磁性固相萃取 高效液相色谱 农药残留 柑橘类水果 

分 类 号：O657.72[理学—分析化学] TS255.7[理学—化学]