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

黄斯敏 胡玉斐 陈彦龙 李攻科 夏凌

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

  • 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。

English


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  • 收稿日期:  2020-06-19
  • 修回日期:  2020-08-04
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