A multiclass
analytical method to determine pesticides and mycotoxins
in beer-related matrices based on the dilute and shoot approach was
optimized and validated according to the European guidelines SANTE/12682/2019
and EC/401/2006. Extraction used acidified acetonitrile at 1% (v/v)
acetic acid, followed by horizontal shaking homogenization, centrifugation,
freeze-out step for cleanup, another centrifugation, and injection
into a high-performance liquid chromatography–tandem mass spectrometry
system. Linearity, detection and quantification limits, accuracy,
and measurement uncertainty were evaluated, and 201, 184, and 176
analytes were validated for malt, beer, and brewers’ spent
grain, respectively. The limits of quantification ranged between 1
and 200 μg kg–1 and between 5 and 1000 μg
kg–1 for beer and malt, respectively, and expanded
uncertainties ranged between 9.7 and 50%, meeting the legislation
requirements. A total of 40 samples have been analyzed thus far, and
36 of them exhibited the presence of some of the analyzed substances.
The validated method is reliable and easy to apply for mycotoxin and
pesticide determination in complex matrices.