It has been established that the antibiotic pefloxacin (Abaktal) methanesulphonate reacts with Fe(III) at pH 1.00-8.00 to form a water-soluble complex with maximum absorbance at 360 nm. The composition of the complex, determined spectrophotometrically by the application of Job's, molar-ratio and Bent-French's methods, was pefloxacin: Fe(III) = 1:1 (pH = 2.50; lambda = 360 nm; mu = 0.1 M). The relative stability constant, obtained by the methods of Sommer and Asmus was 10(5.02) (pH = 2.50; lambda = 360 nm; mu = 0.1 M). The molar absorptivity of the complex at 360 nm was found to be 4.8 x 10(3) l mol-1 cm-1. Beer's law was followed for pefloxacin concentrations of 2.15-85.88 micrograms ml-1. The lower sensitivity limit of the method was 2.15 micrograms ml-1. The relative standard deviation (n = 10) was 0.57-1.07%. The method can be applied to the rapid and simple determination of pefloxacin in aqueous solutions and tablets.