A new voltammetric method for a direct determination of gold nanoparticles, based on adsorption and electrochemical detection of colloidal gold, is described. In this protocol, the absorption of gold nanoparticles onto the rough surface of graphite-epoxy composite electrode is followed by their electrochemical oxidation in 0.1M HCl medium at a potential of +1.25V. The resulting tetrachloroaurate ions generated near the electrode surface are detected by differential pulse voltammetry (DPV). The DPV response is linear in the range from 4.7×10 8 to 4.7×10 11 nanoparticlescm −3 with a limit of detection of 1.8×10 8 gold nanoparticlescm −3 . The surface characteristics of the composite electrode are investigated and the parameters that affect the complete analytical detection process of gold nanoparticles are optimized.