In this work, the voltammetric behavior of melamine was investigated on a nanoparticles modified electrode. The Fe2O3 nanoperticles were prepared and characterized. The melamine showed well defined anodic peak current on the modified electrode. The electro-oxidation was studied in phosphate buffer solution of pH 6.0. The effect of scan rate, volume of suspension and pH were studied for the title reaction. Further, linear sweep voltammetry was used to develop a method to detect melamine. Under optimized conditions, the peak current was linear with the concentration in the range 50 to 160 μM. The limit of detection of 10.5 μM and limit of quantification of 35.5 μM was obtained. Using this optimized method, melamine was detected in commercial milk powder successfully.