The purpose of this research is to develop an electrochemical sensor in order to determine paracetamol (PC) levels. To reach this objective, an indium tin oxide (ITO) electrode was modified with a composite of carbon nanosphere (CNS) and iron-doped bismuth vanadate nanoparticles (Fe0.05Bi0.95VO4), which was tested to evaluate its electrocatalytic properties for the anodic oxidation of PC. Exploiting their various structural advantages that include large exposed active surface sites, ultrathin nanosheets, and unique three-dimensional spherical nanostructure, the as-obtained hybrid electrode Fe0.05Bi0.95VO4/CNS exhibits an excellent electrochemical performance. The fabricated nanocomposite electrode Fe0.05Bi0.95VO4/CNS/ITO reacted rapidly with enhanced anodic peak current when PC analyte is added. At optimized conditions, the proposed electrochemical platform enabled a linear plot over a concentration range of 1–80 μM with a detection limit of 1 μM of PC. This research’s novelty consists of designing a new and effective electrochemical sensing system that can identify PC with high sensitivity and selectivity, helping to keep water quality under control and preventing negative effects on the environment and public health.