Nanostructured copper hexacyanidoferrate has been synthesized and characterized using elemental analysis, atomic absorption spectroscopy, thermal and infrared spectral studies. The transmission electron microscopic studies of the synthesized material showed that it consisted of irregular oval and rod shaped particles with a size range 70-100 nm. Nanostructured copper hexacyanidoferrate modified glassy carbon electrode was characterized by cyclic voltammetery and nanostructured copper hexacyanidoferrate-carbon nanotube composite material modified glassy carbon electrode has been used for electrocatalytic oxidation of salbutamol. The electrode modified with composite material was found to reduce the peak potential of oxidation of salbutamol by nearly 90 mV.