Development and validation of an analytical method for the extraction, identification, and quantification of multi-mycotoxins in beer using a modified QuEChERS procedure and UHPLC-MS/MS

ABSTRACT

Although beer is one of the most popular alcoholic beverages in the world, there is no specific legislation regarding contaminants, especially mycotoxins, for this product. The present manuscript reports the development and validation of an analytical methodology based on the QuEChERS approach, followed by quantification via UHPLC-MS/MS for the simultaneous determination of seventeen mycotoxins in beer. During the validation, amatrix effect was observed for 82% of the analytes. Linearity and recovery were evaluated using spiked blank samples, and the chosen methodology proved to be efficient for all analytes, with recoveries ranging from 71 to 118%, excepting ergonovine, for which recovery of 57% was achieved. Precision was estimated in terms of repeatability and reproducibility, with variations from 2.6 to 28.2% and 9.7 to 28.7%, respectively. The detection (LOD) and quantification (LOQ) limits, determined from the values of CCα and CCβ, ranged from 0.26 to 117 µgkg⁻¹ and from 0.30 to 135 µgkg⁻¹, respectively. Measurement uncertainties were based on the bottom-up methodology, with uncertainties ranging from 0.03 to 17 µgkg⁻¹. Finally, thirty-eight beer samples, collected at the local market, were analysed, and 16 of them showed contamination by deoxynivalenol in concentrations ranging from 159 ± 26 µgkg⁻¹ to 648 ± 106 µgkg⁻¹.

KEYWORDS:

• Food security
• multi-mycotoxins
• validation
• salt-assisted liquid-liquid extraction
• beer

Conflicts of Interest

The authors declare no conflict of interest.

Supplementary material

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Additional information

Funding

This research did not receive external funding.