Isolation and purification of deoxynivalenol and a new trichothecene by high pressure liquid chromatography

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Abstract
Deoxynivalenol (3,7,15‐trihydroxy‐12,l3‐epoxytrichothec‐9‐ene‐8‐one) was extracted from corn with methanol/water (80:20, v/v) and purified by liquid:liquid partitioning and by preparative high pressure liquid chromatography (HPLC). This procedure was used to prepare mg quantities of toxin from field‐inoculated corn for reference standards. Analysis of the isolated deoxynivalenol by analytical HPLC, gas liquid chromatography (GLC) and gas liquid chromatography/mass spectroscopy (GLC/MS) indicated the presence of a second compound similar to deoxynivalenol. This compound comigrates with deoxynivalenol on thin layer chromatography plates in chloroform/methanol (90:10, v/v), but can be separated by HPLC on a reverse‐phase C8 column with methanol/water (10:90, v/v). GC/MS of the compound and the trimethylsilyl ether derivative gave parent ions of m/e 280 and 424, respectively. These data and NMR data indicate that the compound is 3,15‐dihydroxy‐12,13‐epoxytrichothec‐9‐ene‐8‐one, a previously unreported trichothecene.