A method for the quantitative determination of the toxic fungal products diacetoxyscirpenol and T-2 toxin is described. Initially intended for the screening of fungal cultures grown on maize, it has subsequently been used successfully for the analysis of maize and oat grain samples. The method involves extraction with aqueous methanol followed by a two-stage clean-up procedure utilizing a commercial kieselguhr column and a silica gel cartridge. The heptafluorobutyryl derivatives of the trichothecenes, including neosolaniol monoacetate used as an internal standard, are separated on a 25 m X 0.32 mm SE-30 fused silica capillary column and measured with a 63Ni electron capture detector. The quantitative detection limit was found to be of the order of 200 ng/g (ppb) with an average recovery from maize of 88% for both toxins. The method was found to be rapid and practical with the advantage that the kieselguhr packing material could be easily regenerated and re-used. The method was compared with those reported in the literature which are currently in use.