A thin layer chromatographic (TLC) method for determining deoxynivalenol (DON) in corn and wheat was developed. DON is extracted from the grain with acetonitrile–water (84 + 16) and filtered through a column of mixed alumina–charcoal–Celite (0.5 g + 0.7 g + 0.3 g). The solvent is evaporated on a steam bath. Ethyl acetate is added to the residue and heated to dissolve DON. After cooling, the residue is transferred to a vial with additional ethyl acetate and is dissolved in CHCl3–acetonitrile (4 + 1) for TLC on an AlCl3-impregnated silica gel plate with CHCI3–acetone–isopropanol (8 + 1 + 1). The plate is heated in a 120°C oven for 7 min; a blue fluorescent spot is produced under longwave ultraviolet light. DON is quantitated visually and/or fluorodensitometrically by comparison with reference standards. The minimum detectable amount of DON is ca 20 ng/spot. The limit of DON determination is ca 40 ng/g for wheat and 100 ng/g for corn. Recoveries of DON added to wheat and corn at 100, 500, and 1000 ng/ g levels were 85, 93, and 88% and 77, 80, and 80%, respectively.