Abstract: A method was developed for the determination of Ciprofloxacin Hydrochloride and Enrofloxacin in Caviar by high performance liquid chromatography with fluorescence detection.The homogenized sample was extracted with methanol and acidified acetonitrile.The extract was concentrated by nitrogen,and redissolved into 2mL mobile phase and defatted with n-hexane.Ciprofloxacin Hydrochloride and Enrofloxacin were separated on Eclipse XDBC18 Column with mobile phases containing acetonitrile and 0.02 mol·L-1 oxalic acid(14∶86)and finally determined by fluorescence Detector.The detection limit of Ciprofloxacin Hydrochloride and Enrofloxacin were 1μg·kg-1 and 0.5μg·kg-1,separately.In the range of 5-120μg·kg-1,the mean recoveries were more than 80%.The intraday and interday precisions were less than 5%.It showed that this accurate and sensitive method could be applied for the conventional residue testing requirements.