Dispersive liquid-liquid microextraction (DLLME) was combined for the first time with NACE-UV for the selective determination of eight fluoroquinolone antibiotics (lomefloxacin, levofloxacin, marbofloxacin, ciprofloxacin, sarafloxacin, enrofloxacin, danofloxacin and difloxacin) in mineral and run-off waters. Field-enhanced sample injection was carried out in order to improve the sensitivity, whereas pipemidic acid was used as internal standard. The BGE that provided complete separation of the eight analytes and the internal standard was composed of 3 M acetic acid, 49 mM ammonium acetate in 55:45 v/v methanol:ACN. Optimum DLLME conditions (extraction of 5 mL of water at pH 7.6 with 685 μL of CHCl(3) and 1250 μL of ACN, extractant and disperser solvents, respectively) were achieved by means of experimental design methodology. Calibration curves of the whole method were obtained with correlation coefficients (R) higher than 0.994 in all cases. An accuracy and precision study was carried out at different levels of concentration, finding that there were no significant differences (Student's t-test) between real and spiked concentrations.