Mycotoxin Analysis in Foods by SFE-SFC-MS

Importance of the Topic

Mycotoxins are low molecular weight toxins produced by fungi capable of causing severe health issues including carcinogenic and acute toxicity. Ensuring food safety requires rapid reliable methods to detect multiple mycotoxins in diverse food matrices. Traditional approaches rely on labor intensive sample pretreatment steps reducing throughput.

Objectives and Study Overview

This study aimed to develop a fully automated online extraction and analysis workflow for simultaneous detection of key mycotoxins in food samples. The approach combines supercritical fluid extraction with supercritical fluid chromatography and tandem mass spectrometry to streamline sample handling and analysis.

Methodology

Certified reference materials of mycotoxin contaminated peanut butter and multi toxin corn were selected. Samples were weighed and loaded into extraction vessels. Peanut butter was mixed with an absorbent material before extraction. Online supercritical fluid extraction was conducted using carbon dioxide modified with methanol under static and dynamic phases. Extracts were directly transferred to a phenyl bonded column for chromatographic separation employing a gradient of methanol in CO2. Target analytes were monitored by multiple reaction monitoring in the mass spectrometer.

Instrumentation

The workflow was implemented on a Shimadzu Nexera UC system featuring CO2 and modifier pumps degassing units an autosampler column oven back pressure regulators and a triple quadrupole mass spectrometer operated in electrospray mode.

Main Results and Discussion

Standard solutions of eight mycotoxins yielded clear chromatographic peaks at 100 nanogram levels demonstrating baseline separation and detection sensitivity. Analyses of certified reference materials agreed with certified values for aflatoxins except fumonisins which were not analyzed. Aflatoxin G2 was not detected in peanut butter as expected. The method delivered accurate quantitation and reduced sample preparation time.

Benefits and Practical Applications

• Elimination of offline sample pretreatment reduces labor and potential losses
• High throughput simultaneous screening of multiple mycotoxins
• Direct online integration improves reproducibility and reduces contamination risk

Future Trends and Applications

Future developments may include extension to additional toxin classes such as fumonisins and ochratoxins miniaturization of extraction vessels to lower solvent consumption and integration of high resolution mass analyzers for untargeted screening. Implementation in regulatory and quality control laboratories can enhance safety monitoring workflows.

Conclusion

The online SFE SFC MS method on the Nexera UC platform provides a rapid reliable solution for simultaneous mycotoxin analysis in complex food matrices reducing sample preparation and delivering results consistent with certified standards.

References

• Cayman chemical Mycotoxin Standards
• Sigma Aldrich Aflatoxin Reference Material
• Trilogy Analytical Laboratory Multitoxin Corn Reference