Simple, rapid, accurate and sensitive spectrofluorimetric methods for the determination of norfloxacin are described. The methods are based on the reaction of this drug with aluminium(III) ion to form a strongly fluorescent complex. Fluorescence properties of the AlIII-norfloxacin complex were used for the determination of this drug in pharmaceutical preparations. First-derivative constant wavelength synchronous fluorescence spectrometry was used for the determination of norfloxacin in the presence of nalidixic acid. The determination of norfloxacin in urine without the need of tedious pre-separation was achieved by using zero-crossing second-derivative synchronous fluorescence spectrometry.