Analytical Strategies for the Determination of Deoxynivalenol and its Modified Forms in Beer: A Mini Review
Scientific articles | 2015 | Kvasny PrumyslInstrumentation
Deoxynivalenol (DON) is a common Fusarium mycotoxin contaminating cereal crops and end‐products such as beer. Its modified forms, including deoxynivalenol‐3‐β‐D‐glucoside (D3G) and acetylated derivatives (3ADON, 15ADON), may persist through malting and brewing and pose similar health risks. Continuous monitoring of these compounds in beer is essential to assess dietary exposure, support food safety regulations, and protect consumer health.
This mini‐review summarizes current analytical approaches for quantifying DON and its main conjugates in beer. The focus is on the range of instrumental techniques employed, challenges in sample preparation, and the performance characteristics of each method. Immunochemical screening tools are also discussed as rapid alternatives for routine monitoring.
Sample preparation strategies aim to remove complex matrix components and concentrate analytes for low‐level detection (<5 µg/L). Key clean‐up procedures include solid‐phase extraction (SPE), immunoaffinity chromatography (IAC), QuEChERS, and protein precipitation.
Instrumental methods achieve limits of detection suitable for beer analysis: GC-MS and UHPLC-MS/MS reach LOQs below 5 µg/L for DON, while high-resolution MS methods require extensive pre‐concentration to detect modified forms. Multi-analyte LC-MS/MS protocols can simultaneously quantify DON, D3G and 3ADON with recoveries of 60–110% and relative standard deviations below 15%. ELISAs offer high throughput but may overestimate levels due to cross‐reactivity with conjugates and matrix interferences. Comparative evaluations show that matrix-matched calibration or stable isotope‐labeled internal standards are essential to correct signal suppression or enhancement.
Advancements in miniaturized, high‐resolution MS and online sample clean‐up aim to streamline workflows and reduce analysis time. Emerging immunosensors and biosensors may offer point‐of‐use detection. Further research on human bioavailability of masked DON conjugates will inform safety standards and encourage development of multiplexed assays tailored to evolving regulatory requirements.
Effective monitoring of deoxynivalenol and its modified forms in beer requires a combination of robust sample preparation and appropriate analytical techniques. While LC-MS/MS remains the gold standard for quantification, ELISA-based assays are valuable for rapid screening. Future method development should focus on simplifying workflows, improving throughput, and enhancing accuracy for comprehensive risk assessment.
GC, GC/MSD, HPLC, LC/MS
IndustriesFood & Agriculture
ManufacturerSummary
Analytical Strategies for the Determination of Deoxynivalenol and Its Modified Forms in Beer: A Mini Review
Importance of the Topic
Deoxynivalenol (DON) is a common Fusarium mycotoxin contaminating cereal crops and end‐products such as beer. Its modified forms, including deoxynivalenol‐3‐β‐D‐glucoside (D3G) and acetylated derivatives (3ADON, 15ADON), may persist through malting and brewing and pose similar health risks. Continuous monitoring of these compounds in beer is essential to assess dietary exposure, support food safety regulations, and protect consumer health.
Objectives and Study Overview
This mini‐review summarizes current analytical approaches for quantifying DON and its main conjugates in beer. The focus is on the range of instrumental techniques employed, challenges in sample preparation, and the performance characteristics of each method. Immunochemical screening tools are also discussed as rapid alternatives for routine monitoring.
Methodology and Instrumentation
Sample preparation strategies aim to remove complex matrix components and concentrate analytes for low‐level detection (<5 µg/L). Key clean‐up procedures include solid‐phase extraction (SPE), immunoaffinity chromatography (IAC), QuEChERS, and protein precipitation.
Equipment and Techniques
- Gas Chromatography: GC-FID, GC-ECD, GC-MS with derivatization (TMS or HFB) for volatile derivatives
- Liquid Chromatography: HPLC-UV at 220 nm for single-analyte methods, UHPLC-MS/MS for multi‐mycotoxin panels
- Mass Spectrometry: Triple quadrupole MS for targeted quantification; high-resolution Orbitrap and Time-of-Flight MS for non‐targeted screening and structural elucidation
- Immunoassays: ELISA kits (e.g., Ridascreen®, Veratox®, AgraQuant®) for rapid screening without extensive sample clean-up
Main Results and Discussion
Instrumental methods achieve limits of detection suitable for beer analysis: GC-MS and UHPLC-MS/MS reach LOQs below 5 µg/L for DON, while high-resolution MS methods require extensive pre‐concentration to detect modified forms. Multi-analyte LC-MS/MS protocols can simultaneously quantify DON, D3G and 3ADON with recoveries of 60–110% and relative standard deviations below 15%. ELISAs offer high throughput but may overestimate levels due to cross‐reactivity with conjugates and matrix interferences. Comparative evaluations show that matrix-matched calibration or stable isotope‐labeled internal standards are essential to correct signal suppression or enhancement.
Benefits and Practical Applications
- Instrumental methods provide high sensitivity and specificity for confirmatory analysis in quality control, regulatory compliance, and research studies.
- ELISA kits enable rapid screening of large sample sets with minimal equipment, supporting on‐site or high‐throughput workflows.
- Hybrid HRMS approaches facilitate the discovery of novel masked mycotoxins and retrospective data mining without prior knowledge.
Future Trends and Potential Applications
Advancements in miniaturized, high‐resolution MS and online sample clean‐up aim to streamline workflows and reduce analysis time. Emerging immunosensors and biosensors may offer point‐of‐use detection. Further research on human bioavailability of masked DON conjugates will inform safety standards and encourage development of multiplexed assays tailored to evolving regulatory requirements.
Conclusion
Effective monitoring of deoxynivalenol and its modified forms in beer requires a combination of robust sample preparation and appropriate analytical techniques. While LC-MS/MS remains the gold standard for quantification, ELISA-based assays are valuable for rapid screening. Future method development should focus on simplifying workflows, improving throughput, and enhancing accuracy for comprehensive risk assessment.
References
- Malachová A., Varga E., Schwartz‐Zimmermann H. E., Berthiller F. (2015) Analytical strategies for the determination of deoxynivalenol and its modified forms in beer: A mini review. Kvasny Prum., 61(2): 46–50.
- Lancová K., et al. (2008) Transfer of Fusarium mycotoxins and ‘masked’ deoxynivalenol from field barley through malt to beer. Food Addit. Contam. A, 25(6): 732–744.
- Varga E., et al. (2013) Survey of deoxynivalenol and its conjugates in 374 beer samples. Food Addit. Contam. A, 30(1): 137–146.
- Zachariášová M., et al. (2012) Deoxynivalenol oligoglycosides in malt, beer and bread. J. Agric. Food Chem., 60(36): 9280–9291.
- Romero‐Gonzáles R., Aguilera‐Luiz M. M., Frenich A. G. (2009) Multi‐mycotoxin analysis in beers by UHPLC‐MS/MS. J. Agric. Food Chem., 57(20): 9385–9392.
- Papadopoulou‐Bouraoui A., et al. (2004) Screening survey of deoxynivalenol in beer by ELISA. Food Addit. Contam., 21(6): 607–617.
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