食品科学 ›› 2025, Vol. 46 ›› Issue (20): 337-344.doi: 10.7506/spkx1002-6630-20250422-185

• 安全检测 • 上一篇    下一篇

磁性共价有机骨架材料结合HPLC-MS/MS方法用于坚果中真菌毒素的富集与检测

王绘超,于江风,许秀丽,张峰,廉洁   

  1. (1.中国人民公安大学侦查学院,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)
  • 出版日期:2025-10-25 发布日期:2025-09-17
  • 基金资助:
    公安部重点实验室开放基金资助项目(2023-KLDMC-02); 中国人民公安大学刑事科学技术双一流创新研究专项(2023SYL06)

Magnetic Covalent Organic Framework Material Combined with HPLC-MS/MS for the Enrichment and Detection of Mycotoxins in Nuts

WANG Huichao, YU Jiangfeng, XU Xiuli, ZHANG Feng, LIAN Jie   

  1. (1. School of Investigation, 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)
  • Online:2025-10-25 Published:2025-09-17

摘要: 本研究使用2,3-二羟基对苯二甲醛(2,3-dihydroxyterephthalaldehyde,BDD)与邻联甲苯胺(o-tolidine,OT)合成一种新型共价有机骨架材料(covalent organic framework,COF)——Fe3O4@COF(OT-BDD),并将其应用于磁固相萃取过程,同时结合高效液相色谱-串联质谱法,实现坚果中4 种黄曲霉毒素(aflatoxins,AFs)的高效检测。结果显示,AFs分析方法在0.1~100 μg/kg范围内线性关系良好,R2>0.999,加标回收率在86.1%~104.2%之间,日内、日间精密度的相对标准偏差均小于11.2%,方法检出限为0.05~0.12 μg/kg,定量限为0.13~0.37 μg/kg。本研究制备的COF对AFs吸附能力强,适用于坚果中AFs的快速、准确、高灵敏检测,可有效弥补传统AFs检测方法难以应对坚果类食品基质复杂的问题。

关键词: 共价有机骨架材料;黄曲霉毒素;磁固相萃取;坚果

Abstract: In this study, a novel covalent organic framework material, Fe3O4@COF(OT-BDD), was synthesized using 2,3-dihydroxyterephthalaldehyde (BDD) and o-tolidine (OT). This material was applied in magnetic solid phase extraction (MSPE) coupled with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) for the efficient determination of four types of aflatoxins (AFs) in nut samples. The experimental results showed that the developed analytical method exhibited excellent linearity over the concentration range from 0.1 to 100 μg/kg, with determination coefficients (R2) exceeding 0.999. Recovery rates for spiked sample ranged from 86.1% to 104.2%, and intra- and inter-day precisions, expressed as relative standard deviations (RSDs), were less than 11.2%. The limits of detection (LODs) ranged from 0.05 to 0.12 μg/kg, and the limits of quantification (LOQs) ranged from 0.13 to 0.37 μg/kg. The COF material synthesized in this study exhibited strong adsorption capacity for Afs and enabled rapid, accurate, and sensitive detection of AFs in nut samples, effectively addressing the limitations of traditional methods in handling the complex matrix of nut-based food products.

Key words: covalent organic frameworks; aflatoxins; magnetic solid phase extraction; nuts

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