Analysis of Mycotoxins in Food Matrices Using the Agilent Ultivo Triple Quadrupole LC/MS

Significance of the topic

Mycotoxins are harmful fungal metabolites that often contaminate crops and pose serious health risks to humans and livestock. Accurate, sensitive detection of these compounds in food matrices is critical to comply with regulatory limits and safeguard public health.

Objectives and Study Overview

This study presents a robust LC–MS/MS method using the Agilent Ultivo triple quadrupole system to quantify 12 regulated mycotoxins in corn and peanut matrices and five in black pepper. The goal was to achieve detection limits well below the maximum levels established by EU Regulations 1881/2006 and 105/2010, while streamlining lab workflow and instrument footprint.

Methodology and Sample Preparation

Sample preparation involved:

• Weighing 5 g of corn or peanuts (2 g for black pepper).
• Extraction with 10 mL acetonitrile and 10 mL water containing 0.2% formic acid.
• QuEChERS EN salt addition, vortex mixing, and centrifugation.
• Dilution of supernatants and cleanup using Agilent Captiva EMR–Lipid cartridges.

LC separation was performed on an Agilent Eclipse Plus C18 column (3.0 × 150 mm, 1.8 µm) at 45 °C with a methanol–water gradient containing ammonium fluoride, ammonium formate, and formic acid. Detection used positive-mode dynamic MRM on the Ultivo system.

Instrumentation

• Agilent 1290 Infinity II UHPLC (high-speed pump G7120A, multisampler G7167B, column thermostat G7116B).
• Agilent Ultivo Triple Quadrupole LC/MS with Jet Stream ESI source.
• Agilent MassHunter Quantitative Analysis B.09 software.

Main Results and Discussion

The method exhibited:

• Limits of quantitation at or below 1/5 of assigned MLs for all mycotoxins.
• Recoveries between 60% and 110% at ML levels across different matrices.
• Precision with %RSD ≤10% (most <5%) at LOQ in all matrices.
• Linearity with correlation coefficients (R2) ≥0.99 over 1/20 to 10× ML concentration ranges.

Benefits and Practical Applications

The compact design of the Ultivo system reduces bench space and maintenance time, enabling high throughput and reliable performance in food safety and QA/QC laboratories. The combined sample cleanup and advanced MS detection support routine monitoring of mycotoxins in diverse food commodities.

Future Trends and Potential Applications

Emerging directions include expansion of compound panels, integration with automated sample handling, and development of targeted screening for new mycotoxins. Miniaturized, high-throughput LC–MS platforms will further enhance real-time monitoring and on-site testing capabilities.

Conclusion

The Agilent Ultivo triple quadrupole LC/MS method delivers sensitive, precise, and rapid quantification of multiple mycotoxins well below regulatory limits, supporting stringent food safety requirements in a compact, user-friendly system.

References

• Bennett, J. W.; Klich, M. Mycotoxins. Clinical Microbiology Reviews 2003, 16(3), 497–516.
• Commission Regulation (EC) No 1881/2006 Setting maximum levels for certain contaminants in foodstuffs. Official Journal of the European Union 2006, L 364/5–24.
• Commission Regulation (EU) No 105/2010 Amending Regulation (EC) No 1881/2006 as regards ochratoxin A. Official Journal of the European Union 2010, L 35/7–8.