Analytical Strategies for the Determination of Deoxynivalenol and its Modified Forms in Beer: A Mini Review

Importance of the Topic

Deoxynivalenol (DON) is a prevalent Fusarium mycotoxin that poses significant health risks to consumers. Modified forms such as deoxynivalenol-3-β-D-glucoside (D3G) and acetylated derivatives (3ADON, 15ADON) can co-occur and survive malting and brewing processes, leading to measurable levels in beer. Reliable analytical strategies are essential to ensure product safety and regulatory compliance.

Objectives and Study Overview

This mini-review summarizes current methods for detecting DON and its modified forms in beer. It evaluates gas chromatography (GC) with various detectors, liquid chromatography (LC) with ultraviolet (UV) and mass spectrometric detection, high-resolution MS approaches, and immunochemical assays. Emphasis is placed on sample preparation, method performance, and suitability for routine monitoring.

Applied Methodology and Instrumentation

Sample preparation techniques include:

• Solid-phase extraction (SPE) and immunoaffinity chromatography (IAC) for clean-up and concentration
• QuEChERS protocols combining acetonitrile extraction, salting out, and dispersive SPE
• Liquid–liquid partitioning and simple ‘‘dilute and shoot’’ approaches

Instrumental platforms cover:

• GC with flame ionization detection (FID), electron capture detection (ECD), and GC-MS after derivatization
• HPLC/UHPLC with UV detection at 220 nm and tandem mass spectrometry (MS/MS) using ESI or APCI
• Ultra-high-performance LC coupled to triple quadrupole and high-resolution MS (Orbitrap, time-of-flight)
• Enzyme-linked immunosorbent assays (ELISA) for rapid screening

Main Results and Discussion

GC-based methods achieve low limits of detection (0.5–2 µg/L) but require laborious derivatization and extensive clean-up. HPLC-UV methods with IAC clean-up reach quantification limits around 5–10 µg/L. LC-MS/MS assays offer superior sensitivity (LOD ≤1 µg/L) and multiplexing capability but demand careful control of matrix effects, often via matrix-matched calibration or stable-isotope dilution. High-resolution MS enables non-targeted screening of masked forms but at higher cost and LODs around 3–5 µg/L. ELISA kits allow fast analysis (<30 min) but may overestimate DON due to cross-reactivity with conjugates and matrix interferences.

Benefits and Practical Applications of the Method

Advanced LC-MS/MS and HRMS techniques support simultaneous multi-mycotoxin profiling and retrospective data mining. Immunochemical assays facilitate high-throughput screening in quality control laboratories. Validated protocols have been applied in large-scale surveys, demonstrating frequent co-occurrence of DON and D3G in commercial beers and informing risk assessments.

Future Trends and Opportunities

Emerging approaches include stable-isotope dilution assays for accurate quantification, improved immunoaffinity materials for masked mycotoxin enrichment, and enhanced HRMS workflows for discovery of novel conjugates such as DON oligoglycosides. Integration of rapid screening with confirmatory MS methods and expansion of occurrence data will support regulatory guidelines for DON and its derivatives in beer.

Conclusion

Reliable detection of DON and modified forms in beer relies on a balance between sensitivity, throughput, and cost. LC-MS/MS with tailored sample preparation remains the gold standard, while ELISA offers efficient pre-screening. Continued method development and harmonized validation will enhance consumer safety and industry compliance.

Reference

Anselme M et al. Food Addit Contam A 2006; Berthiller F et al. Mol Nutr Food Res 2013; Lancová K et al. Food Addit Contam A 2008; Malachová A et al. World Mycotoxin J 2012; Zachariášová M et al. Rapid Commun Mass Spectrom 2010