食品科学 ›› 2024, Vol. 45 ›› Issue (20): 263-269.doi: 10.7506/spkx1002-6630-20240511-086

• 安全检测 • 上一篇    下一篇

共价有机框架材料磁性固相萃取结合高效液相色谱-串联质谱法检测茶叶中黄曲霉毒素

赵东岳, 许秀丽, 王秀娟, 吴薇, 张峰   

  1. (1.中国检验检疫科学研究院食品安全研究所,北京 100176;2.青岛农业大学食品科学与工程学院,山东 青岛 266109;3.山东省产品质量检验研究院,山东 济南 250100)
  • 出版日期:2024-10-25 发布日期:2024-10-14
  • 基金资助:
    检科院工作经费项目

Determination of Aflatoxins in Tea by Magnetic Solid Phase Extraction Based on Covalent Organic Framework Coupled with High Performance Liquid Chromatography-Tandem Mass Spectrometry

ZHAO Dongyue, XU Xiuli, WANG Xiujuan, WU Wei, ZHANG Feng   

  1. (1. Institute of Food Safety, Chinese Academy of Inspection and Quarantine, Beijing 100176, China; 2. School of Food Science and Engineering, Qingdao Agricultural University, Qingdao 266109, China; 3. Shandong Institute for Product Quality Inspection, Jinan 250100, China)
  • Online:2024-10-25 Published:2024-10-14

摘要: 建立了一种基于共价有机框架材料的磁性固相萃取(magnetic solid phase extraction,M-SPE)结合高效液相色谱-串联质谱(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)方法,用于茶叶中4 种黄曲霉毒素(aflatoxins,AFs)的高效测定。样品经过乙腈、水和冰醋酸按8.0∶1.9∶0.1(V/V)提取、离心、M-SPE和过滤,净化后滤液经正离子模式测定,并用HPLC-MS/MS法进行定量。建立的4 种AFs分析方法在0.05~50 μg/L范围内线性良好,决定系数R2>0.999 2,加标回收率在67.6%~103.7%之间,日内、日间精密度均小于9.24%,方法检出限为0.01~0.06 μg/kg,定量限为0.05~0.20 μg/kg。本研究制备的共价有机框架材料对AFs吸附能力强,开发的M-SPE-HPLC-MS/MS适用于茶叶中AFs的快速、高灵敏、准确检测。

关键词: 共价有机框架材料;高效液相色谱-串联质谱;黄曲霉毒素;磁固相萃取

Abstract: A magnetic solid phase extraction (M-SPE) based on covalent organic framework materials coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for the efficient determination of four aflatoxins (AFs) in tea. The samples were extracted with a mixture of acetonitrile, water and glacial acetic acid (8.0:1.9:0.1, V/V) and centrifuged. The supernatant was evaporated to almost dryness, re-dissolved in water and pH adjusted, extracted M-SPE and filtered, and the filtrate was detected in the positive ion mode. The calibration curves for all analytes were linear in the range of 0.05–50 μg/L with coefficients of determination (R2) > 0.999 2, the spiked recoveries were in the range of 67.6%-103.7%, and the relative standard deviations (RSDs) for intra- and inter-day precisions were less than 9.24%, the limits of detection (LODs) were in the range of 0.01-0.06 μg/kg, and the limits of quantification (LOQs) of the developed method were in the range of 0.05-0.20 μg/kg. The covalent organic framework material prepared in this study has a strong adsorption capacity for AFs, and M-SPE-HPLC-MS/MS is suitable for the rapid, highly sensitive and accurate detection of AFs in tea.

Key words: covalent organic framework materials; high performance liquid chromatography-tandem mass spectrometry; aflatoxin; magnetic solid phase extraction

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