食品科学 ›› 2022, Vol. 43 ›› Issue (4): 315-320.doi: 10.7506/spkx1002-6630-20201231-364

• 安全检测 • 上一篇    下一篇

QuEChERS结合UPLC-Q/Orbitrap HRMS法测定小麦粉中9 种真菌毒素

齐春艳,许秀丽,国伟,李翔,吴玉平   

  1. (1.中国检验检疫科学研究院,北京 100176;2.广东省食品检验所(广东省酒类检测中心),广东 广州 510000)
  • 出版日期:2022-02-25 发布日期:2022-03-08
  • 基金资助:
    国家市场监督管理总局技术保障专项(2019YJ061)

Determination of Nine Mycotoxins in Wheat Flour by QuEChERS-Ultra-high Performance Liquid Chromatography-Quadrupole/Orbitrap High-Resolution Mass Spectrometry

QI Chunyan, XU Xiuli, GUO Wei, LI Xiang, WU Yuping   

  1. (1. Chinese Academy of Inspection and Quarantine, Beijing 100176, China; 2. Guangdong Institue of Food Insepction (Guangdong Inspection Center of Wine and Spirits), Guangzhou 510000, China)
  • Online:2022-02-25 Published:2022-03-08

摘要: 建立QuEChERS-高效液相色谱-四极杆/静电轨道离子阱高分辨质谱法同时测定小麦粉中9 种真菌毒素的方法。样品经2.0%甲酸-乙腈提取,QuEChERS盐包脱水盐析后,用dSPE净化管净化,超高效液相色谱分离,在正离子模式下进行检测。在全扫描模式下测定目标化合物的一级精密质量数,与理论精密质量数相比,相对偏差不大于1.91×10-6,可实现精准定性;同时建立了9 种真菌毒素的二级质谱数据库,实现对9 种真菌毒素的定性筛查及同步定量。9 种真菌毒素线性范围为0.25~100 μg/L,定量限范围为0.30~3.00 μg/kg,在低、中、高3 个不同添加水平下的平均回收率为70.2%~112.0%,相对标准偏差为0.2%~4.5%。该方法可作为小麦粉中真菌毒素的高通量筛查和确认检测方法。

关键词: 小麦粉;真菌毒素;QuEChERS;高效液相色谱-四极杆/静电轨道离子阱高分辨质谱

Abstract: A method was developed for the simultaneous determination of nine mycotoxins in wheat flour by ultra-high performance liquid chromatography-quadrupole/orbitrap high-resolution mass spectrometry (UPLC-Q/Orbitrap HRMS) combined with QuEChERS (quick, easy, cheap, effective, rugged and safe) pretreatment. Samples were extracted with acetonitrile/formic acid solution (98.0:2.0, V/V), salted out with a QuEChERS salt pocket, and then purified with a dispersive solid phase extraction (dSPE) tube. The target compounds were separated by UPLC and detected in the positive ion mode. Measured accurate mass-to-charge ratios of the nine mycotoxins were obtained in the full scan mode with a relative deviation not more than 1.91 × 10-6 compared to the theoretical value, indicating accurate qualitative analysis of these compounds. A tandem mass spectral library for simultaneous screening and quantitation of the mycotoxins was built based on characteristic fragment ions. The linear ranges were 0.25–100 μg/L for all target analytes. The limit of quantification (LOQ) ranged from 0.30 to 3.00 μg/kg. Average recoveries at three spiked levels were in the range of 70.2%-112.0% with relative standard deviation (RSD) of 0.2%–4.5%. This method is useful for the high-throughput screening and confirmation of mycotoxins in wheat flour.

Key words: wheat flour; mycotoxins; QuEChERS; ultra-high performance liquid chromatography-quadrupole/orbitrap high-resolution mass spectrometry

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