Analytical techniques for determination of mycotoxins in barley, malt and beer: A review

Analytical Techniques for Determination of Mycotoxins in Barley Malt and Beer A Review

Significance of the Topic

The reliable determination of mycotoxins in barley malt and beer is critical for ensuring consumer safety and meeting strict regulatory limits. Mycotoxins such as aflatoxins deoxynivalenol ochratoxin A and zearalenone may contaminate cereals during cultivation storage or processing and transfer into malt and beer. Accurate analysis protects public health supports quality control in malting and brewing and underpins international trade.

Study Objectives and Overview

This review aimed to summarize the current analytical methods for detecting mycotoxins in barley malt and beer. Key goals included describing sample preparation strategies extraction and clean-up procedures and surveying instrumental techniques from classical chromatography to modern mass spectrometry and rapid immunochemical assays.

Methodology and Instrumentation

Sample Preparation and Clean-Up

• Sampling and homogenization to address heterogeneous mycotoxin distribution
• Extraction solvents commonly acetonitrile–water mixtures with acidified water to improve recovery
• Clean-up by solid-phase extraction immunoaffinity columns or dispersive methods such as QuEChERS to reduce matrix effects

Instrumental Techniques

• Liquid chromatography coupled with fluorescence or ultraviolet detection and tandem mass spectrometry (LC–MS/MS) for high sensitivity multi-mycotoxin analysis
• Gas chromatography–mass spectrometry (GC–MS) often with derivatization for volatile mycotoxins
• Thin layer chromatography (TLC) and enzyme-linked immunosorbent assay (ELISA) for screening purposes
• Rapid biosensors and spectroscopic methods including near-infrared (NIR) and Raman techniques for preliminary screening

Instrumentation Used

• HPLC and UPLC systems with photodiode array fluorescence and UV detectors
• Triple quadrupole and ion trap mass spectrometers with ESI APCI and APPI interfaces
• Immunoaffinity columns and magnetic molecularly imprinted polymers for selective clean-up
• Solid phase extraction and QuEChERS kits for multi-residue preparation

Main Results and Discussion

The review highlights that LC–MS/MS is the method of choice for simultaneous quantification of over 30 mycotoxins with limits of detection typically in the low microgram per kilogram range. QuEChERS extraction with minimal clean-up enables broad toxin coverage but requires matrix-matched calibration or isotope dilution to correct signal suppression. Immunoaffinity clean-up combined with HPLC-FLD remains widely used for specific toxins like ochratoxin A. Rapid screening by ELISA NIR or Raman spectroscopy can flag contaminated lots for confirmatory analysis.

Benefits and Practical Applications

Well validated chromatographic methods ensure compliance with EU and international mycotoxin limits and support quality control throughout the brewing supply chain. Rapid screening assays enable high throughput monitoring at intake warehouses malt plants and breweries to prevent contaminated batches from entering production. Multi-mycotoxin LC–MS/MS protocols reduce analysis time and cost by covering diverse toxins in a single run.

Future Trends and Potential Applications

Advances in high-resolution mass spectrometry and multiplexed biosensors will further improve sensitivity and throughput. Portable spectroscopic devices and lab-on-chip biochips promise in situ mycotoxin screening at field and processing sites. Molecularly imprinted polymers and magnetic nanomaterials offer selective clean-up for emerging toxins and masked metabolites. Integration of data analytics and predictive modeling with routine testing could anticipate outbreaks and optimize harvest and storage practices.

Conclusion

The analysis of mycotoxins in barley malt and beer has evolved from simple screening assays to sophisticated multi-residue LC–MS/MS methods. Robust sampling extraction and clean-up protocols combined with advanced detection ensure that regulatory limits are met and consumer safety is maintained. Ongoing innovations in rapid screening and selective extraction will further strengthen quality control in the brewing industry.

References

• Pernica M Piacentini KC Benešová K Čáslavský J Běláková S Analytical techniques for determination of mycotoxins in barley malt and beer A review Kvasny prumysl 2019 65 46–57
• Anastassiades M Lehotay SJ Štajnbaher D Schenck FJ Fast and easy multiresidue method employing acetonitrile extraction and dispersive solid-phase extraction for pesticide residues in produce JAOCS 2003 86 2 412–431
• Pereira VL Fernandes JO Cunha SC Mycotoxins in cereals and related foodstuffs A review of occurrence and analysis Trend Food Sci Technol 2014 36 96–136
• Rubert J Soler C Marín R James KJ Mañes J Mass spectrometry strategies for mycotoxin analysis in European beers Food Control 2013 30 122–128
• Turner NW Subrahmanyam S Piletsky SA Analytical methods for determination of mycotoxins a review Anal Chim Acta 2009 632 2 168–180