Abstract The selective determination of norfloxacin in mixtures with other fluorquinolones was achieved by synchronous scanning solid surface room-temperature phosphorimetry (SSRTP) and Th(NO 3) 4 as selective phosphorescence inducer. The method also allowed the determination of levofloxacin in a sequential way. The optimization of experimental conditions was made through an univariate approach, in order to find the best conditions for norfloxacin phosphorescence, followed by a 2 3 factorial design in order to verify interaction among relevant variables, to check robustness for each variable and to perform final adjustment of parameters. Absolute limit of detection (ALOD) for norfloxacin was 12 ng with a linear signal response extending up to 400 ng. Under the same experimental conditions set for norfloxacin, the ALOD for levofloxacin was 13 ng with linear signal response up to 450 ng. Accuracy of the method, using Th (IV) as selective phosphorescence inducer, was evaluated through the analysis of commercial and simulated pharmaceutical formulations with recoveries between 94.4 and 101% for norfloxacin and 95.9 and 103.8% for levofloxacin. The use of Cd (II), a traditional phosphorescence inducer for fluorquinolones, did not allow selective determination of norfloxacin. Further studies indicated the potential application of the method in urine samples.