The Co3O4/CuO composite nanopowder (NP) was synthesized by a mechanochemical method and characterized by using powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and energy-dispersive spectroscopy (EDS). The synthesized Co3O4/CuO NP was used as a modified carbon paste electrode (MCPE) and further the bare carbon paste and Co3O4/CuO NP modified carbon paste was heated at different temperatures (100, 150, 200 and 250°C) for 10min. The Co3O4/CuO NP MCPE was used to study the consequences of scan rate and dopamine concentration. Furthermore the preheated modified electrodes were used to study the electrochemical response to dopamine (DA), ascorbic acid (AA) and uric acid (UA).