Two Cu (II) complexes, [Cu (L1)2] (NO3) 2 (1) and [Cu (L2)2] (NO3)2 (2), which L1 and L2 Schiff base ligands are 2- (thiophene-2-yl) -1 H imidazo [4, 5-f] [1, 10] phenanthroline and 2- (furane-2-yl) -1 H imidazo [ 4, 5-f] [1, 10] phenenthroline, respectively, were synthesized and characterized by physico - chemical and spectroscopic methods. Corresponded CuO nanoparticles were prepared by calcination of the obtained complexes at 500oC. The structure of nano sized copper oxides were characterized by X- ray diffraction (XRD) and scanning electron microscopy (SEM). Electrocatalytic oxidation of acetylcholine (ACh) on copper oxide nanostructures were investigated. The results showed that acetylcholine (ACh) was oxidized irreversibly on copper oxide nanostructures with an excellent catalytic activity.