混合模式固相萃取-高效液相色谱法测定牛奶中4种非甾体抗炎药残留

丁健桦 徐文平 朱玉玲

引用本文: 丁健桦, 徐文平, 朱玉玲. 混合模式固相萃取-高效液相色谱法测定牛奶中4种非甾体抗炎药残留[J]. 分析化学, 2023, 51(6): 1013-1023. doi: 10.19756/j.issn.0253-3820.211239 shu
Citation:  DING Jian-Hua,  XU Wen-Ping,  ZHU Yu-Ling. Mixed-mode Solid Phase Extraction Coupled with High Performance Liquid Chromatography for Analysis of Non-steroidal Anti-inflammatory Drugs Residues in Bovine Milk[J]. Chinese Journal of Analytical Chemistry, 2023, 51(6): 1013-1023. doi: 10.19756/j.issn.0253-3820.211239 shu

混合模式固相萃取-高效液相色谱法测定牛奶中4种非甾体抗炎药残留

    通讯作者: 朱玉玲,E-mail:zyl9568@ecut.edu.cn
  • 基金项目:

    江西省科技厅重点研发计划项目(No.20192BBG7008)和东华理工大学博士科研启动基金项目(No.DHBK2019145)资助。

摘要: 制备了咪唑离子液体功能化的混合模式硅胶吸附剂(Sil-IL),将其作为固相萃取(SPE)吸附剂,结合高效液相色谱-紫外检测方法(HPLC-UV),建立了测定牛奶中酮洛芬、萘普生、吲哚美辛和托芬那酸4种非甾体类抗炎药物(NSAIDs)的分析方法。通过红外光谱、拉曼光谱和元素分析对Sil-IL进行了表征,初步探索了Sil-IL对目标物的保留作用机理,考察了样品溶液的pH值、上样流速、淋洗液及洗脱溶剂体积等因素对SPE效率的影响。结果表明,Sil-IL对4种NSAIDs的保留主要通过疏水作用和阴离子交换作用,Sil-IL吸附剂对4种NSAIDs具有较好的萃取选择性和萃取效率。在优化的SPE条件下,托芬那酸的线性检测范围为4~1000 μg/L,其它3种NSAIDs的线性范围为3~1000 μg/L,相关系数(R2)为0.9996~0.9998,检出限为1.2~1.9 μg/kg(S/N=3),日内和日间精密度分别为1.0%~3.0%和1.9%~6.3%,加标回收率为90.8%~105.3%。本方法准确可靠、灵敏度高、背景干扰低小、操作简便,可用于奶制品中4种NSAIDs残留的同时检测。

English


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  • 收稿日期:  2021-03-21
  • 修回日期:  2023-05-29
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