CAPILLARY GAS-LIQUID-CHROMATOGRAPHIC DETERMINATION OF VOMITOXIN IN CEREAL-GRAINS

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  • 1 January 1982
    • journal article
    • research article
    • Vol. 65  (6) , 1429-1434
Abstract
A GLC method, using an electron capture detector, was described for determining vomitoxin in cereal grains at levels as low as 0.05 pm. Samples were extracted with chloroform-ethanol and initially purified by using A Sep-Pak silica cartridge, followed by column chromatography using Sephadex LH-20. Additional purification was achieved using a disposable cyano cartridge. Heptafluorobutyrylimidazole (HFBI) was added to form esters of the analytes. The HFB esters of vomitoxin were separated on a 30 m .times. 0.25 mm fused silica column coated with SE-54 and measured with a 63Ni electron capture detector. Samples were confirmed by GLC/mass spectrometry using electron impact ionization and single ion monitoring at the molecular ion mass of 884.05 and at 10,000 resolving power. The method was applied to wheat, oats, barley and corn. The limit of detection was 0.05 ppm vomitoxin. Average recoveries were 89.8% with a coefficient of variation of 4.0%.

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