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Article

Development and Validation of an UHPLC-MS/MS Method for the Simultaneous Determination of 11 EU-Regulated Mycotoxins in Selected Cereals

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Department of Food Technology, University North, Trg Dr. Žarka Dolinara 1, 48000 Koprivnica, Croatia
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Inspecto Ltd., Industrijska Zona Nemetin, Vukovarska Cesta 239b, 31000 Osijek, Croatia
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Faculty of Food Technology, Josip Juraj Strossmayer University of Osijek, Franje Kuhača 18, 31000 Osijek, Croatia
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Polytechnic in Požega, Vukovarska 17, 34000 Požega, Croatia
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CROTEH—Sustainable Technologies Development Centre Ltd., Dragutina Golika 63, 10000 Zagreb, Croatia
*
Author to whom correspondence should be addressed.
Academic Editor: Julio Alberto Zygadlo
J. Fungi 2022, 8(7), 665; https://doi.org/10.3390/jof8070665
Received: 24 May 2022 / Revised: 17 June 2022 / Accepted: 21 June 2022 / Published: 24 June 2022
The availability of reliable sensitive multi-analyte methods for unambiguous determination of mycotoxins is crucial for ensuring food and feed safety, considering their adverse health effects and (co-)occurrence in various foods. Accordingly, a multi-mycotoxin confirmatory method for simultaneous determination of 11 mycotoxins regulated in cereals within the European Union (EU) using ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) was developed and in-house validated to fit the EU legislation requirements for analytical methods. A simple sample preparation was based on a solid–liquid extraction using a solvent mixture acetonitrile/water/formic acid (79/20/1, v/v/v) and a dilution of raw extract using water/acetonitrile/formic acid (79/20/1, v/v/v) before instrumental analysis. Average recoveries in all three validated cereal crop types (maize, wheat, and barley), spiked at multiple levels, were found acceptable for all analytes when matrix-matched calibration was used, ranging from 63.2% to 111.2% and also showing very good repeatability, with relative standard deviations below 20%. Matrix effect (SSE) evaluation revealed maize as the most complex of the three analyzed cereal matrices, with strong SSE (<50% and >150%) recorded for all 11 analyzed mycotoxins. An additional method verification was performed through successful participation in proficiency testing schemes, with the achieved z-scores generally in the acceptable range of −2 ≤ z ≤ 2. The obtained validation results demonstrated the suitability of the developed confirmatory multi-mycotoxin UHPLC-MS/MS method based on a dilute-and-shoot principle for the simultaneous determination of low concentrations of 11 EU-regulated mycotoxins in cereals, including aflatoxins B1, B2, G1 and G2, deoxynivalenol, fumonisins B1 and B2, zearalenone, T-2 and HT-2 toxins, and ochratoxin A. View Full-Text
Keywords: food and feed safety; cereals; multi-mycotoxin analysis; UHPLC-MS/MS; method performance food and feed safety; cereals; multi-mycotoxin analysis; UHPLC-MS/MS; method performance
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MDPI and ACS Style

Kovač, M.; Nevistić, A.; Kovač, T.; Babić, J.; Šarić, A.; Miličević, B.; Panjičko, M.; Šarkanj, B. Development and Validation of an UHPLC-MS/MS Method for the Simultaneous Determination of 11 EU-Regulated Mycotoxins in Selected Cereals. J. Fungi 2022, 8, 665. https://doi.org/10.3390/jof8070665

AMA Style

Kovač M, Nevistić A, Kovač T, Babić J, Šarić A, Miličević B, Panjičko M, Šarkanj B. Development and Validation of an UHPLC-MS/MS Method for the Simultaneous Determination of 11 EU-Regulated Mycotoxins in Selected Cereals. Journal of Fungi. 2022; 8(7):665. https://doi.org/10.3390/jof8070665

Chicago/Turabian Style

Kovač, Marija, Ante Nevistić, Tihomir Kovač, Jurislav Babić, Antonija Šarić, Borislav Miličević, Mario Panjičko, and Bojan Šarkanj. 2022. "Development and Validation of an UHPLC-MS/MS Method for the Simultaneous Determination of 11 EU-Regulated Mycotoxins in Selected Cereals" Journal of Fungi 8, no. 7: 665. https://doi.org/10.3390/jof8070665

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