色谱

色谱 ›› 2020, Vol. 38 ›› Issue (7): 782-790.DOI: 10.3724/SP.J.1123.2019.10034

• 研究论文 • 上一篇    下一篇

加速溶剂萃取-QuEChERS-超高效液相色谱-串联质谱法测定药食同源性食品中16种真菌毒素

方真1, 曲栗1, 古淑青1,*(), 陈柔含2, 李优1, 邓晓军1, 郭德华1, 冯峰3   

  1. 1 上海海关动植物与食品检验检疫技术中心, 上海 200135
    2 上海大学生命科学学院食品工程系, 上海 200436
    3 中国检验检疫科学研究院, 北京 100176
  • 收稿日期:2019-10-30 出版日期:2020-07-08 发布日期:2020-12-10
  • 通讯作者: 古淑青
  • 作者简介:古淑青.Tel:38620526, E-mail:gushuqing@sina.cn
  • 基金资助:
    国家重点研发计划项目(2017YFF0211003);上海市科委项目(19395810100);上海市科委项目(19391901500);上海市科委项目(17DZ2201200)

Determination of 16 mycotoxins in drug and food homologous products by ultra performance liquid chromatography-tandem mass spectrometry combined with accelerated solvent extraction and QuEChERS

FANG Zhen1, QU Li1, GU Shuqing1,*(), CHEN Rouhan2, LI You1, DENG Xiaojun1, GUO Dehua1, FENG Feng3   

  1. 1 Technical Center for Animal Plant and Food Inspection and Quarantine, Shanghai Customs, Shanghai 200135, China
    2 Department of Food Engineering, School of Life Science, Shanghai University, Shanghai 200436, China
    3 Chinese Academy of Inspection and Quarantine, Beijing 100176, China
  • Received:2019-10-30 Online:2020-07-08 Published:2020-12-10
  • Contact: GU Shuqing
  • Supported by:
    National Key Research and Development Plan Project(2017YFF0211003);Shanghai Science and Technology Commission Project(19395810100);Shanghai Science and Technology Commission Project(19391901500);Shanghai Science and Technology Commission Project(17DZ2201200)

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摘要：

建立了加速溶剂萃取-QuEChERS-超高效液相色谱-串联质谱测定药食同源性食品中16种真菌毒素的方法。样品经过加速溶剂萃取后用QuEChERS方法净化，液相色谱分离，在正、负离子同时扫描和多反应离子监测模式下检测，黄曲霉毒素B1和伏马毒素B1采用内标法定量，其余毒素采用基质外标法定量。在较宽的线性范围内，16种目标化合物的线性相关系数（r2）均大于0.99。该方法的检出限为0.008~0.3 μg/kg，定量限为0.03~1.0 μg/kg，在3个不同添加水平下的加标回收率为70.8%~118%，RSD为2.5%~10.2%。采用建立的方法分别对市面上销售的30个批次的山银花、葛根和沙棘产品进行检测，部分产品检出不同含量的真菌毒素。该方法快速、灵敏，适用于药食同源性食品中多种真菌毒素的同时检测。

关键词: 超高效液相色谱-串联质谱, 加速溶剂萃取, QuEChERS, 真菌毒素, 药食同源性食品

Abstract:

A method was developed for the simultaneous determination of 16 mycotoxins in drug and food homologous products by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) combined with accelerated solvent extraction (ASE) and QuEChERS. The target mycotoxins in drug and food homologous products were extracted by ASE. After concentration, the extracts were purified by QuEChERS. Then, the target compounds were analyzed by UPLC-MS/MS in both positive and negative electrospray ionization and MRM modes. Aflatoxin B1 and fumonisin B1 were quantified by the internal standard method, and the remaining mycotoxins were quantified by the matrix-matched external standard method. The proposed method showed a good linear relationship, with correlation coefficients greater than 0.99. The limits of detection (LODs) and limits of quantification (LOQs) of the 16 mycotoxins ranged from 0.008 μg/kg to 0.3 μg/kg and from 0.03 μg/kg to 1.0 μg/kg, respectively. The blank samples were spiked at three levels, and the recoveries ranged from 70.8% to 118%, with the RSDs being 2.5% to 10.2%. The developed method was successfully applied to mycotoxin analysis in 30 scutellaria, puerarin and sea buckthorn samples bought from local markets. Different levels of mycotoxins were detected in some of the products. The proposed method is simple, rapid and sensitive, and it can be applied to the simultaneous determination of multi-mycotoxins in drug and food homologous products.

Key words: ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), accelerated solvent extraction (ASE), QuEChERS, mycotoxins, drug and food homologous products