食品科学 ›› 2026, Vol. 47 ›› Issue (1): 291-300.doi: 10.7506/spkx1002-6630-20250717-148

• 安全检测 • 上一篇    

磁性分子印迹聚合物固相萃取-超高效液相色谱-串联质谱法测定花生和酱油中4 种黄曲霉毒素

任玉龙,王秀娟,邵振超,庞博,廉洁,许秀丽   

  1. (1.中国人民公安大学 刑事科学技术北京市重点实验室,北京 100038;2.中国质量检验检测科学研究院食品安全研究所,北京 100176)
  • 发布日期:2026-02-04
  • 基金资助:
    刑事科学技术北京市重点实验室建设项目(2023ZB06)

Magnetic Molecularly Imprinted Polymer-Based Solid-Phase Extraction Combined with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry for the Determination of Four Aflatoxins in Peanuts and Soy Sauce

REN Yulong, WANG Xiujuan, SHAO Zhenchao, PANG Bo, LIAN Jie, XU Xiuli   

  1. (1. Beijing Key Laboratory of Criminal Science and Technology, People’s Public Security University of China, Beijing 100038, China; 2. Institute of Food Safety, Chinese Academy of Quality and Inspection & Testing, Beijing 100176, China)
  • Published:2026-02-04

摘要: 建立一种基于磁性分子印迹聚合物(Fe3O4@MIP)的磁固相萃取(magnetic solid-phase extraction,MSPE)结合超高效液相色谱-串联质谱(ultra-high performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)新方法,用于花生和酱油中4 种黄曲霉毒素(aflatoxins,AFs)的快速、高灵敏度测定。采用表面接枝聚合策略,以5,7-二甲氧基香豆素为虚拟模板,甲基丙烯酸为功能单体,乙二醇二甲基丙烯酸酯为交联剂,成功制备对AFs具有选择性的Fe3O4@MIP。随后,系统优化MSPE萃取条件。结果表明,该方法在0.02~100 μg/kg含量范围内线性关系良好(R2>0.991 5),在花生基质中的加标回收率在87.63%~103.58%之间,日内和日间精密度的相对标准偏差均低于8.16%,方法的检出限低至0.006 9~0.011 μg/kg。所制备的Fe3O4@MIP对AFs展现出优异的选择性和可重复使用性。本研究开发的MSPE-UPLC-MS/MS方法操作简便、灵敏度高,能有效克服基质干扰,为复杂食品中痕量AFs的快速、准确检测提供了可靠方案,在食品安全监控领域具有重要的应用价值。

关键词: 分子印迹;超高效液相色谱-串联质谱;黄曲霉毒素;磁固相萃取

Abstract: This study established a new method using magnetic solid-phase extraction (MSPE) based on a novel magnetic molecularly imprinted polymer (Fe3O4@MIP) combined with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for the rapid and sensitive determination of four aflatoxins (AFs) in peanuts and soy sauce. Using a surface grafting polymerization strategy, Fe3O4@MIP with selectivity for AFs was successfully prepared with 5,7-dimethoxycoumarin as a dummy template, methacrylic acid (MAA) as a functional monomer, and ethylene glycol dimethacrylate (EGDMA) as a cross-linker. Subsequently, the MSPE extraction conditions were systematically optimized. The results showed that the developed method had good linearity within the concentration range of 0.02–100 μg/kg (R2 > 0.991 5), with spiked recoveries in the peanut matrix ranging from 87.63% to 103.58%. Both intra-day and inter-day precision (relative standard deviation (RSD)) were below 8.16%, and the limit of detection (LOD) was as low as 0.006 9–0.011 μg/kg. The prepared Fe3O4@MIP exhibited excellent selectivity and reusability for AFs. The MSPE-UPLC-MS/MS method is simple to operate and highly sensitive, and can effectively overcome matrix interferences, providing a reliable solution for the rapid and accurate detection of trace AFs in complex foods, and holding significant application value in the field of food safety monitoring.

Key words: molecular imprinting; ultra-high performance liquid chromatography-tandem mass spectrometry; aflatoxins; magnetic solid-phase extraction

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