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Article Dans Une Revue Food Additives and Contaminants Année : 2009

LC-MS/MS multi-analyte method for mycotoxin determination in food supplements

Sofie Monbaliu
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Marie-Louise Scippo
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Guy Maghuin-Rogister
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Yves-Jacques Schneider
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Yvan Larondelle
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Alfons Callebaut
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Johan Robbens
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Carlos van Peteghem
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Sarah de Saeger
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Résumé

A multi-analyte method for the liquid chromatography-tandem mass spectrometric determination of mycotoxins in food supplements is presented. The analytes included A and B trichothecenes (nivalenol, deoxynivalenol, 3-acetyldeoxynivalenol, 15-acetyldeoxynivalenol, neosolaniol, fusarenon-X, diacetoxyscirpenol, HT-2 toxin and T-2 toxin), aflatoxins (aflatoxin-B1, aflatoxin-B2, aflatoxin-G1 and aflatoxin-G2), Alternaria toxins (alternariol, alternariol methyl ether and altenuene), fumonisins (fumonisin-B1, fumonisin-B2 and fumonisin-B3), ochratoxin A, zearalenone, beauvericin and sterigmatocystin. Optimization of the simultaneous extraction of these toxins and of the sample pre-treatment procedure, as well as method validation were performed on maca (Lepidium meyenii) food supplements. The results indicated that the solvent mixture ethyl acetate/formic acid (95:5, v/v) is the best compromise for the extraction of the analytes from food supplements. Liquid-liquid partition with n-hexane was applied as partial clean-up step to remove excess of co-extracted non-polar components. Further clean-up was performed on Oasis HLBTM cartridges. Samples were analysed using an Acquity UPLC system coupled to a Micromass Quattro Micro triple quadrupole mass spectrometer equipped with an electrospray interface operated in the positive ion mode. Limits of detection and quantification were in the range of 0.3-30 ng/g and 1-100 ng/g, respectively. Recovery yields were above 60 % for most of analytes, except for nivalenol, sterigmatocystine and the fumonisins. The method showed good precision and trueness. Analysis of different food supplements such as soy (Glycine max) isoflavones, St John's wort (Hypericum perforatum), garlic (Allium sativum), Ginkgo biloba and black radish (Raphanus niger) demonstrated the general applicability of the method. Due to different matrix effects observed in different food supplement samples, the standard addition approach was applied to perform correct quantitative analysis. In 56 out of 62 samples analyzed none of the 23 mycotoxins investigated was detected. Positive samples contained at least one of the toxins fumonisin-B1, fumonisin-B2, fumonisin-B3 and ochratoxin A.

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Dates et versions

hal-00573883 , version 1 (05-03-2011)

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José Diana Di Mavungu, Sofie Monbaliu, Marie-Louise Scippo, Guy Maghuin-Rogister, Yves-Jacques Schneider, et al.. LC-MS/MS multi-analyte method for mycotoxin determination in food supplements. Food Additives and Contaminants, 2009, 26 (06), pp.885-895. ⟨10.1080/02652030902774649⟩. ⟨hal-00573883⟩

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