Uric acid, a metabolite formed by the oxidation of purines in the human body, plays a crucial role in disease development when its metabolism is altered. Various techniques have been employed for uric acid analysis, with electrochemical sensing emerging as a sensitive, selective, affordable, rapid, and simple approach. In this study, we developed a polymer-based sensor (PPy/α-Fe2O3) for the accurate determination of uric acid levels. The PPy/α-Fe2O3 hybrids were synthesized using an uncomplicated in situ growth technique. Characterization of the samples was performed using scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), X-ray powder diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). The electrochemical sensing performance towards uric acid was evaluated through cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The obtained results demonstrated that the sensor exhibited excellent sensitivity towards uric acid detection within a wide range of 5–200 μM with a limit of detection (LOD) as low as 1.349 μM. Furthermore, this work elucidated the underlying sensing mechanism and highlighted the pivotal role played by PPy/α-Fe2O3 hybrids in enabling efficient uric acid sensing applications using electrochemical sensors.