The detection and quantification of mycotoxins in beer are critical for ensuring consumer safety and regulatory compliance. These contaminants, originating from barley and other grains, persist and potentially transform during the brewing process. This study presents an innovative analytical protocol using liquid chromatography/electrospray ionization tandem mass spectrometry (HPLC/ESI-MS/MS) for the simultaneous qualitative and quantitative analysis of nine mycotoxins, including aflatoxins (AFB1, AFB2, AFG1, AFG2), Ochratoxin A (OTA), Fumonisins (FB1, FB2), Deoxynivalenol (DON), and HT-2. The method leverages the efficiency of multi-mycotoxin immunoaffinity columns, providing streamlined sample preparation with high specificity and sensitivity. Validation was conducted using craft beers from Calabria, including freeze-dried samples to enhance analytical consistency and stability. The method’s accuracy was confirmed by using spiking samples with mycotoxins at concentrations compliant with the European Commission’s regulations (Recommendation 2024/1038/EU). The developed protocol delivers reliable results with minimized resource consumption, offering a robust tool for quality control and safety assessments in brewing. By addressing knowledge gaps in freeze-dried craft beer, this study contributes to advancing food safety standards in the brewing industry.

In this study, a UHPLC-PDA method for the simultaneous identification of polyphenols and bitter acids (alpha, beta, and isoalpha) in beer was developed. The resulting chemical profiles were leveraged to distinguish the characteristics of four (IPA, Lager, Blanche, ALE) bergamot-flavored beers, produced on a pilot-scale plant. In a streamlined 29 min analysis, thirty polyphenols and fourteen bitter acids were successfully identified under optimized separation conditions. Validation, encompassing parameters such as LOD (from 0.028 ppm for isorhamnetin to 0.106 for narirutin), LOQ (from 0.077 ppm for naringenin to 0.355 for narirutin), R² (always more than 0.9992), repeatability (from 0.67% for tangeretin to 6.38% for myricetin), and reproducibility (from 0.99% for sinensetin to 6% for naringin), was conducted for polyphenol quantification using constructed calibration curves with seven levels. Exploring polyphenolic components as potential discriminators among different beer styles, a total of thirty-two polyphenolic compounds were identified and quantified, including characteristic bergamot peel polyphenols like neoeriocitrin (from 7.85 ppm for CBS2 to 11.95 ppm in CBS1); naringin (from 4.56 ppm for CBS4 to 10.96 in CBS1), and neohesperidin (from 5.93 in CBS3 to 15.95 for CBS2). The multivariate analysis provided additional insights into variations among specific beer styles, revealing discrepancies in the presence or relative concentrations of specific compounds linked to brewing ingredients and processes. This research enhances the fingerprinting of the chemistry governing beer quality through a straightforward and cost-effective analytical approach.

The detection and quantification of mycotoxins in beer are critical for ensuring consumer safety and regulatory compliance. These contaminants, originating from barley and other grains, persist and potentially transform during the brewing process. This study presents an innovative analytical protocol using liquid chromatography/electrospray ionization tandem mass spectrometry (HPLC/ESI-MS/MS) for the simultaneous qualitative and quantitative analysis of nine mycotoxins, including aflatoxins (AFB1, AFB2, AFG1, AFG2), Ochratoxin A (OTA), Fumonisins (FB1, FB2), Deoxynivalenol (DON), and HT-2. The method leverages the efficiency of multi mycotoxins immunoaffinity columns, providing streamlined sample preparation with high specificity and sensitivity. Validation was conducted using craft beers from Calabria, including freeze-dried samples to enhance analytical consistency and stability. The method's accuracy was confirmed by spiking samples with mycotoxins at concentrations compliant with the European Commission's regulations (Recommendation 2024/1038/EU). The developed protocol delivers reliable results with minimized resource consumption, offering a robust tool for quality control and safety assessments in brewing. By addressing knowledge gaps in freeze-dried craft beer, this study contributes to advancing food safety standards in the brewing industry.

This study outlines the development of an innovative method utilizing UHPLC-PDA for the simultaneous identification of polyphenols and bitter acids (alpha-acids, beta-acids, and iso-alpha-acids) in beer samples. The resulting chemical profiles were leveraged to distinguish the characteristics of four bergamot-flavored beers, each representing distinct styles (IPA, Lager, Blanche, and ALE), produced on a pilot-scale plant. In a streamlined 29-minute analysis, twenty-nine polyphenols and fourteen bitter acids were successfully identified under optimized separation conditions. Rigorous validation, encompassing parameters such as Limit of Detection (LOD), Limit of Quantification (LOQ), R-squared (R2), repeatability, and reproducibility, was conducted for polyphenol quantification using constructed calibration curves with seven levels. Exploring polyphenolic components as potential discriminators among different beer styles, a total of thirty-two polyphenolic compounds were identified and quantified, including characteristic bergamot peel polyphenols like neoeriocitrin, naringin, and neohesperidin. The determination of bitter units and total phenols further aided in style differentiation. Multivariate analysis provided additional insights into variations among specific beer styles, revealing discrepancies in the presence or relative concentrations of specific compounds linked to brewing ingredients and processes. This research enhances to trace the fingerprinting of the chemistry governing beer quality through a straightforward and cost-effective analytical approach, readily applicable in common laboratories.