A novel procedure using high performance liquid chromatography(HPLC) with fluorescence detector for the determination of thiamphenicol(TAP),florfenicol(FF) and florfenicol amine(FFA) in aquatic products was described.The analytes were extracted by basic ethyl acetate-acetonitril,gel permeation chromatography(GPC) was used for cleanup,excitation and emission wavelength were 225 nm and 295 nm for fluorescence detection.The average recoveries and relative standard deviations(RSDs) for the analysis of all samples fortified over the range of 0.050~2.0 mg/kg were in the range of 86.4%~96.8% and 5.63%~ 9.71%(n=5),respectively.Good linearities were obtained in the concenttration ranging from 0.20~5.0 mg/L for TAP and FF,and 0.10~5.0 mg/L for FFA.The limits of detection were 0.020 mg/kg for TAP and FF,and 0.010 mg/kg for FFA.