A Rapid Single-Extraction Method for the Simultaneous Determination of Aflatoxins B1, B2, G1, G2, Fumonisin B1, and Zearalenone in Corn Meal by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry
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A single-extraction method to simultaneously determine aflatoxins (B1, B2, G1, G2), fumonisin B1, and zearalenone in corn meal by ultra performance liquid chromatography tandem mass spectrometry, using a triple quadrupole, was optimized, validated, and applied in an occurrence study. Different extraction solutions were tested, with better performance for methanol/acetonitrile/water (60:20:20, v/v/v). Linearity was observed from 0.25 to 1.50 ng/mL for aflatoxins, from 20 to 120 ng/mL for fumonisin, and from 7.00 to 42.00 ng/mL for zearalenone. Significant matrix effects were shown for all groups. Selectivity was demonstrated, as matrix or spectral interferences were not observed at the predicted retention time window of the target analytes. Average recoveries of 87.57, 93.18, 93.35, 94.20, 78.76, and 95.98% were obtained for aflatoxins (B1, B2, G1, and G2) fumonisin and zearalenone, respectively. A z-score of 0.19 was estimated in a corn certified reference material for fumonisin B1. Maximum relative standard deviation values under repeatability and intermediate precision conditions were determined to be 13.6 and 13.6% for aflatoxins, 3.7 and 6.3% for fumonisin, and 3.5 and 4.0% for zearalenone, respectively. In the occurrence study, 50 samples were analyzed and 44% had measurable levels of fumonisin. Zearalenone was detected in 18%. The proposed method showed considerable advantages, considering environmental impacts, efficiency, and reliability.
KeywordsMycotoxins Food Mass spectrometry Multigroup determination Single-laboratory validation Application
The authors acknowledge the friends at the Mycotoxins Laboratory of the Ezequiel Dias Foundation and those at the Food Science Laboratory of the Federal University of Minas Gerais. We would also like to thank Waters Technologies in Brazil for their technical support and FAPEMIG for the financial support.
Compliance with Ethical Standards
Conflict of Interest
Fabiano Narciso Paschoal declares that he has no conflict of interest. Daniela de Azevedo Silva declares that she has no conflict of interest. Rafael von Sperling de Souza declares that he has no conflict of interest. Marize Silva de Oliveira declares that she has no conflict of interest. Danilo Augusto Alves Pereira declares that he has no conflict of interest. Scheilla Vitorino Carvalho de Souza declares that she has no conflict of interest.
This article does not contain any studies with human participants or animals performed by any of the authors.
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