Abstract
Here we present a method for simultaneous determination of the fungal metabolites mycophenolic acid, ochratoxin A (OTA) and fumonisin B2 (FB2) in meat products. Extraction was performed with water–acetonitrile, followed by acetone-induced precipitation of salts and proteins. Purification and identification of analytes was performed by mixed-mode reversed-phase anion-exchange chromatography in direct ion-exchange mode, followed by liquid chromatography–tandem mass spectrometry (LC-MS/MS) detection. Quantification was based on isotope dilution with fully 13C-labelled FB2 and OTA, and matrix-spiked calibration curves. Fermented sausages inoculated with an OTA- and FB2-producing strain of Aspergillus niger were analysed, but no analytes were detected. Analysis of 22 retail products showed one Parma meat with a very high level of OTA contamination (56–158 μg/kg) that clearly exceeded the Italian regulatory limit of 1 μg/kg. This sample and uninfected control samples were subsequently reanalysed, and the high OTA content was verified by two other techniques: (i) LC–time-of-flight MS confirmed the accurate mass as well as chlorine isotope pattern; and (ii) sample methylation in methanol–BF3 and subsequent LC-MS/MS provided indirect confirmation by detection of the OTA methyl ester. In the contaminated Parma ham, the high OTA level most likely originated from growth of Penicillium nordicum on the meat.
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Acknowledgements
We are thankful for the supply of raw sausages from the Danish Meat Research Institute. This project was supported by the Danish Meat Association, the Centre for Advanced Food Studies, and the Danish Food Industry Agency (grant 3304-FVEP-07-730-01).
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Sørensen, L.M., Mogensen, J. & Nielsen, K.F. Simultaneous determination of ochratoxin A, mycophenolic acid and fumonisin B2 in meat products. Anal Bioanal Chem 398, 1535–1542 (2010). https://doi.org/10.1007/s00216-010-4059-z
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DOI: https://doi.org/10.1007/s00216-010-4059-z