A simple and sensitive method for the spectrophotometric determination of diosmin has been developed, and optimum reaction conditions along with other analytical parameters have been evaluated. Diosmin, as a phenolic compound, reacts with sodium nitroprusside and hydroxylamine hydrochloride in a basic medium to give a green-colored product. At analytical wavelength of 763 nm, Beer's law is obeyed over the concentration range 2-140 lg mL À1 of diosmin with a correlation coefficient of 0.9997. The molar absorptivity is 9671 L mol À1 cm À1 . The limits of detection (LOD) and quantification (LOQ) are 0.05 and 0.2. lg mL À1 , respectively. The method has been successfully applied to the determination of diosmin in a commercial pharmaceutical preparation. The results were compared favorably with those obtained by the 4-aminoantipyrine method.