New SPE Sorbent for Clean-up of Fusarium Toxin-contaminated Cereals & Cereal-based Foods, Bond Elut Mycotoxin

Importance of the Topic

The presence of Fusarium mycotoxins in cereals and cereal‐based foods poses significant health risks and is subject to strict regulatory limits in many regions. Trichothecenes and zearalenone are among the most prevalent Fusarium toxins, requiring sensitive and reliable analytical methods to ensure food safety and regulatory compliance.

Objectives and Study Overview

This study aimed to develop and validate a streamlined solid‐phase extraction (SPE) cleanup procedure using a novel sorbent, Bond Elut Mycotoxin, for the simultaneous determination of 12 type A and B trichothecenes plus zearalenone in a variety of cereal matrices. The goal was to maximize recoveries—particularly for polar toxins—while minimizing matrix effects and reducing the need for multiple immunoaffinity columns.

Methodology and Instrumentation

• Sample Preparation: 25 g of finely ground cereal sample extracted with 100 mL acetonitrile/water (80/20, v/v) by high‐speed blending for 3 minutes.
• Internal Standard: Zearalanone (ZAN) spiked at 50 ng/g for quantitation of zearalenone (ZEA).
• SPE Cleanup: 4 mL filtered extract passed through Bond Elut Mycotoxin cartridge, eluate evaporated to dryness under nitrogen at 50 °C and reconstituted in acetonitrile/water (20/80, v/v).
• Analysis: 10 µL injected into an LC‐MS/MS system for targeted multi‐analyte quantitation.
• Instrumentation Used: LC‐MS/MS platform coupled with SPE manifold and Bond Elut Mycotoxin cartridges.

Main Results and Discussion

• Recovery Performance: Spiking experiments across wheat, corn, durum, oats, bread, muesli and infant cereal yielded recoveries of 82–100% for most analytes; polar trichothecenes (nivalenol, T-2 tetraol, deoxynivalenol) improved to 66–75%.
• Comparison with Conventional Cleanup: The new sorbent increased polar analyte recoveries by up to 31% versus charcoal–alumina cartridges.
• Naturally Contaminated Samples: Analysis of six real‐world samples showed up to 43% higher levels of polar toxins when using Bond Elut Mycotoxin compared to conventional methods.
• ZEA Quantitation: Use of ZAN as internal standard provided consistent ~100% recovery across all matrices.

Benefits and Practical Applications

• Unified Cleanup: Single SPE sorbent for 13 mycotoxins, eliminating the need for multiple immunoaffinity columns.
• Cost and Time Savings: Simplified workflow and reduced consumable costs.
• Regulatory Compliance: Improved accuracy for QA/QC in food and feed testing laboratories.

Future Trends and Potential Applications

Integration with automated SPE platforms and high‐resolution mass spectrometry may further enhance throughput and selectivity. Expansion to additional mycotoxin classes and miniaturized extraction techniques could support large‐scale monitoring and field applications.

Conclusion

Bond Elut Mycotoxin offers an efficient, cost‐effective SPE cleanup solution for simultaneous determination of multiple Fusarium toxins in cereals. The method enhances recoveries—especially for polar analytes—while meeting stringent regulatory requirements for food safety analysis.

References

1. Langseth W., Rundberget T. (1998) Instrumental methods for determination of nonmacrocyclic trichothecenes in cereals, foodstuffs and cultures. Journal of Chromatography A, 815:103–121.
2. Eriksen G.S., Petterson H., Lundt T. (2004) Comparative cytotoxicity of deoxynivalenol, nivalenol, their acetylated derivatives and de-epoxy metabolites. Food and Chemical Toxicology, 42:619–624.
3. European Commission Scientific Committee on Food (2002) Opinion on Fusarium toxins Part 6: T-2 toxin, HT-2 toxin, nivalenol and deoxynivalenol.
4. Commission Regulation (EC) No. 856/2005 of 6 June 2005 amending Regulation (EC) No. 466/2001 as regards Fusarium toxins.
5. Commission Regulation (EC) No. 401/2006 of 23 February 2006 laying down methods of sampling and analysis for the official control of mycotoxins in foodstuffs.
6. Krska R., Baumgartner S., Josephs R. (2001) The state‐of‐the‐art in the analysis of Type A- and B-trichothecene mycotoxins in cereals. Fresenius Journal of Analytical Chemistry, 371:285–299.
7. Klötzel M., Schmidt S., Lauber U., Thielert G., Humpf H.-U. (2005) Comparison of different clean-up procedures for analysis of deoxynivalenol in cereal-based food and validation of an HPLC method. Chromatographia, 62:41–48.
8. Berthiller F., Schuhmacher R., Buttinger G., Krska R. (2005) Rapid simultaneous determination of major type A- and B-trichothecenes and zearalenone in maize by HPLC-MS/MS. Journal of Chromatography A, 1062:209–216.
9. Klötzel M., Gutsche B., Lauber U., Humpf H.-U. (2005) Determination of 12 Type A- and B-trichothecenes in cereals by LC-ESI-MS/MS. Journal of Agricultural and Food Chemistry, 53:8904–8910.
10. Klötzel M., Lauber U., Humpf H.-U. (2006) A new SPE clean-up method for determination of 12 trichothecenes in cereals and cereal-based food by LC-MS/MS. Molecular Nutrition and Food Research, 50:261–269.