An HPLC method with fluorescence detection is presented for the analysis of enrofloxcin (ENR) and ciprofloxacin (CIP) in chicken tissue using sarafloxacin (SAR) as internal standard. Tissue sample preparations were carried out by adding a phosphate buffer (pH 7.4, 0.1 M), followed by extraction with trichloromethane. Fluoroquinolones were separated on a reversed-phase column with a mobile phase of aqueous phosphate buffer-acetonitrile (80:20). The concentrations of CIP, ENR and SAR eluted off the column, with retention times of 2.28, 3.30 and 4.40, respectively, were monitored by fluorescence detection at )~ex 338 and )~em 425 rim. The detection limitwas 32 ng g 1 forCIPand 10 ng g 1 for ENR. The standard curves were linearly related to concentration in the range of 1 to 2000 ng g 1. Recoverywas determinated as 91.3% and 78.3% for ENR and CIP, respectively. The measurement of the tissue levels of ENR and CIP in the chicken after oral administration confirmed the utility of the proposed analytical methodology.ENR and CIP are recommended for use in a variety of studies.The simultaneous determination of ENR and CIP has been described several times, but always with some clear shortcomings, such as the use of an external standard, time-consuming sample preparation, prolonged elution times or expensive methods [12 15].Against this background, our objective has been to develop a sensitive, rapid and economical HLPC method with fluorescence detection and an internal standard for the simultaneous determination of ENR and its primary metabolite CIP in tissues. In this sense, this method was applied to determine ENR and CIP concentrations in the liver and muscle of chickens after chronic oral administration.