This manuscript explains the effective determination of urea by redox cyclic voltammetric analysis, for which a modified polypyrrole-graphene oxide (PPY-GO, GO 20% w/w of PPY) nanocomposite electrode was developed. Cyclic voltammetry measurements revealed an effective electron transfer in 0.1 M KOH electrolytic solution in the potential window range of 0 to 0.6 V. This PPY-GO modified electrode exhibited a moderate electrocatalytic effect towards urea oxidation, thereby allowing its determination in an electrolytic solution. The linear dependence of the current vs. urea concentration was reached using square-wave voltammetry in the concentration range of urea between 0.5 to 3.0 μM with a relatively low limit of detection of 0.27 μM. The scanning electron microscopy was used to characterize the morphologies and properties of the nanocomposite layer, along with Fourier transform infrared spectroscopy. The results indicated that the nanocomposite film modified electrode exhibited a synergistic effect, including high conductivity, a fast electron-transfer rate, and an inherent catalytic ability.