Quantification of 700 mycotoxins and other secondary metabolites of fungi and plants in grain products

This work reports on the validation of a liquid chromatography-tandem mass spectrometric method for the simultaneous quantification of more than 700 mycotoxins and other secondary fungal metabolites and plant toxins in pasta, biscuits, crackers and musli. The "dilute and shoot" approach was found to be fully applicable to these complex matrices, as only 7–14% of the analytes exhibited significant matrix effects while recoveries of the extraction were outside the target range of 70–120% for only 26 compounds. Data on repeatability (based on 7 brands per matrix) and on intermediate precision was compliant to the related <20% criterion for 95–98% and 99% of all analytes, respectively. The limits of quantification were much lower than the related regulatory limits set for mycotoxins in cereal products. Application of the method to 157 samples from the European market revealed the presence of enniatins and deoxynivalenol in the majority of the samples. No regulatory limits were exceeded except the sum of ergot alkaloids being higher in a few samples than the 50–150 µg/kg to be implemented as of July 2024.

Michael Sulyok, Michele Suman, Rudolf Krska