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用于测定玉米中多种霉菌毒素的超高效液相色谱-飞行时间质谱法:方法开发与验证

UHPLC-ToF-MS method for determination of multi-mycotoxins in maize: Development and validation.

作者信息

Silva Ana Sanches, Brites Carla, Pouca Ana Vila, Barbosa Jorge, Freitas Andreia

机构信息

National Institute for Agricultural and Veterinary Research (INIAV), Rua dos Lágidos, Lugar da Madalena, 4485-655 Vila do Conde, Portugal.

Center for Study in Animal Science (CECA), ICETA, University of Oporto, Oporto, Portugal.

出版信息

Curr Res Food Sci. 2019 Jul 31;1:1-7. doi: 10.1016/j.crfs.2019.07.001. eCollection 2019 Nov.

DOI:10.1016/j.crfs.2019.07.001
PMID:32914099
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC7473352/
Abstract

An Ultra-High Performance Liquid Chromatography combined with Time-of-Flight Mass Spectrometry (UHPLC-ToF-MS) method has been developed for determination of nine mycotoxins, namely aflatoxins (AFB, AFB, AFG and AFG), ochratoxin A (OTA), zearalenone (ZEA), toxin T2 (T2) and fumonisins (FB and FB) in maize. The method included a two-step extraction with acetonitrile 80% (v/v). After optimization, the analytical method was validated. The different concentrations tested take in account the Maximum Levels (ML) for maize (Commission Regulation EC no. 1881/2006) and good results for repeatability (%RSD ≤ 15.4%), reproducibility (%RSD ≤ 15.9%) and recovery (77.8-110.4%, except for AFG2 at 2 μg/kg which presented a recovery of 73.4%) were achieved. These met the performance criteria imposed by Commission Regulation (EC) no. 401/2006. The method was applied to twenty-two samples from Portuguese producers of maize. Fumonisins were the most frequently detected mycotoxins, but the levels do not exceed those imposed by European legislation.

摘要

已开发出一种超高效液相色谱与飞行时间质谱联用(UHPLC-ToF-MS)的方法,用于测定玉米中的九种霉菌毒素,即黄曲霉毒素(AFB₁、AFB₂、AFG₁和AFG₂)、赭曲霉毒素A(OTA)、玉米赤霉烯酮(ZEA)、T-2毒素(T-2)以及伏马毒素(FB₁和FB₂)。该方法包括用80%(v/v)乙腈进行两步萃取。优化后,对该分析方法进行了验证。所测试的不同浓度考虑了玉米的最大限量(欧盟委员会法规EC No. 1881/2006),并在重复性(%RSD≤15.4%)、再现性(%RSD≤15.9%)和回收率(77.8 - 110.4%,2 μg/kg的AFG₂除外,其回收率为73.4%)方面取得了良好结果。这些结果符合欧盟委员会法规(EC)No. 401/2006规定的性能标准。该方法应用于来自葡萄牙玉米生产商的22个样品。伏马毒素是最常检测到的霉菌毒素,但含量未超过欧洲法规规定的水平。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/67e6/7473352/f4e11f01003b/gr2.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/67e6/7473352/f7031590c564/fx1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/67e6/7473352/59a18b9aec44/gr1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/67e6/7473352/f4e11f01003b/gr2.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/67e6/7473352/f7031590c564/fx1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/67e6/7473352/59a18b9aec44/gr1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/67e6/7473352/f4e11f01003b/gr2.jpg

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