Multi-mycotoxin LC-MS/MS method validation and its application to fifty-four wheat flours in Hungary

ABSTRACT

In this study, fifty-four wheat flour and wheat-based products available on the Hungarian market were assessed for twelve mycotoxins. Prior to analysis, a multi-mycotoxin method using high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS) was developed and validated for wheat and wheat-based products. A simple extraction with acetonitrile/water/formic acid (79/20/1 v/v%) was used for sample preparation. The limits of quantitation (LOQ) were between 0.02 and 161 μg kg⁻¹. Good linearity (r² > 0.995) was achieved for all mycotoxins investigated. Recoveries varied between 88 and 120% at three concentration levels. Based on the low relative matrix effect (RSD < 0.15%) of the different wheat flour samples, matrix-matched calibration was used, which also proved its suitability in proficiency testing (z-scores: −0.6 for DON; +1.5 for OTA; −0.5 for ZEA). DON was the predominant mycotoxin, which contaminated 84% of the investigated samples. Metabolised forms of DON were found in spelt, durum flour and some wheat-based products (D3G in 4 samples, 15Ac-DON in 7 samples). T-2 and HT-2 were the second most frequently detected mycotoxins. All investigated samples complied with current European/Hungarian legislation.

KEYWORDS:

• Mycotoxins
• multi-mycotoxin analysis
• HPLC-MS/MS
• wheat flour
• Hungarian wheat flours

Acknowledgments

The Authors would like to acknowledge the financial support of the National Competitiveness and Excellence Program (no. NVKP_16-1-2016-0035), the European Union and the co-financing provided by the European Social Fund (grant agreement no. EFOP3.6.3-VEKOP-16-2017-00005) and the Food Science Doctorial School of SZIU, Hungary. The Authors greatly acknowledge Pál Vágvölgyi for English language editing their manuscript.

Declaration of interest

The authors declare that they have no conflict of interest.

Supplementary material

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