Gas chromatographic determination of deoxynivalenol in cereals
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Summary
Samples of barley, wheat and maize were analysed for deoxynivalenol (DON). Samples were extracted with aqueous chloroform-ethanol. The extract was purified by column chromatography on silica gel. DON was derivatised with heptafluorobutyric (HFB) acid anhydride. The glassware was silylated to prevent deterioration of the HFB derivative, which stabilised the samples for at least 11 weeks. Quantitation was done by capillary gas chromatography using electron-capture detection. Confirmation was obtained by gas chromatography-mass spectrometry. The limit of determination was 0.02 mg/kg. Recoveries of DON averaged 99% with a coefficient of variation of 10.8%.
Keywords
Maize Anhydride Column Chromatography Deoxynivalenol Acid AnhydrideGaschromatographische Bestimmung von Deoxynivalenol in Cerealien
Zusammenfassung
Es wird ein Analyseverfahren zur Bestimmung von Deoxynivalenol (DON) in Roggen, Weizen und Mais beschrieben. Die Proben wurden mit wässerigem Chloroform-Ethanol extrahiert und die Extrakte saulenchromatographisch über Kieselgel gereinigt. Die Derivatisierung wurde mit Heptafluorbuttersäure anhydrid (HFB) durchgefiihrt. Das Glasgerät wurde silyliert, um Zerfall des HFB-Derivats zu verhindern, wodurch die Proben mindestens 11 Wochen stabil waren. Die Bestimmung erfolgte mittels Capillargaschromatographie mit Elektroneneinfangdetektion. Positive Befunde wurden gaschromatographisch-massenspektrometrisch überprüft. Die Bestimmungsgrenze lag bei 0,02 mg/kg. Die Wiederfindungsrate für DON betrug 99% mit einem Variationskoeffizient von 10,8%.
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