Nanostructured ZrO 2 -based materials with their biocompatibility, excellent electrical, and surface charge properties became one of the best candidates for the electrochemical sensing applications. Here, synthesis of Zr 1-x Cu x La x O 2 compounds was achieved in nanoscale and fully characterized using XRD, TEM, DRS, and cyclic voltammetry. A mixture of monoclinic and cubic phases was detected for the undoped ZrO 2 (Z sample, x = 0). For the Cu-doped compounds, (ZFW1, x = 0.05 and ZFW2, x = 0.1), a combination of cubic fluorite and monoclinic phase were detected. The intensity of the monoclinic phase for the Cudoped was higher than that of the undoped ZrO 2 sample. Cu and La co-doped samples (ZL1C1, x = 0.05 and ZL2C2, x = 0.1) were stabilized in a single cubic phase structure. Therefore, their band gap dropped from (4.8 eV) for the undoped ZrO 2 to (1.49 eV) for the ZL1C1 sample and (2 eV) for the ZL2C2 sample. Voltammetric sensing of neurotransmitter metabolites (vanillylmandelic acid (VMA) and homovanillic acid (HVA)) was achieved using the modified electrodes due to their acquired high electrocatalytic and high electrochemical performance.