Zinc hydroxide (Zn(OH)2) nanoparticles with nanocrystal morphology and grain size ~48 nm have been successfully synthesized by using a two-step, template- and surfactant-free method. The synthesized product was characterized by FTIR, powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy-dispersive spectroscopy (EDX). The XRD pattern of zinc oxide confirms formation of the wurtzite structure of Zn(OH)2. For the first time zinc oxide nanostructures have been used for electrocatalytic oxidation and determination of sympathomimetic drugs in aqueous solution. The electrochemical parameters of sympathomimetic drugs were investigated by means of cyclic voltammetry and differential pulse voltammetry as well as flow injection analysis.