A method was developed for the determination of T-2&HT-2 toxin in grains by liquid chromatography with fluorescence detection after immunoaffinity column clean-up and pre-cloumn chemical derivatization. Samples were extracted with methanol-water( 80: 20,v /v),and purified by immunoaffinity columns containing antibodies specific for T-2&HT-2 toxin. Then derived with 1-anthroylnitrile( 1-AN) and 4-dimethylaminopyridine( DMAP). ZORBAX Eclipse XDB-phenyl column and mobile phase of acetonitrile-water were used for analysis. Recoveries from the different cereals spiked with T-2&HT-2 toxin at levels ranging from 0. 005 to 0. 5μg /g were from 82. 0% to 108. 0%,the relative standard deviations were less than 15. 5% and the limit of detection was 0. 005μg /g. This method has a higher clean-up degree,sensitive,stable,low cost and can be applied widely.