This study focuses on the fabrication of a novel electrochemical sensor for ultrasensitive detection of carbofuran, a commonly used carbamate herbicide known for its neurotoxic effects at low doses. A CeO2/NiO/GO nanocomposite was developed using a hydrothermal technique, leveraging cerium's large surface area, ionic conductivity, and wide band gap, which were enhanced by doping with nickel oxide (NiO) and incorporating graphene oxide (GO). Characterization methods, including EDX, SEM, XRD, FTIR, and UV-visible spectroscopy, confirmed the successful production of the nanocomposite. Electrochemical studies using differential pulse voltammetry (DPV), cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS) revealed that CeO2/NiO/GO-modified GCE performed efficiently. The sensor showed a significant increase in oxidation peak current, indicating effective electron transport and carbofuran oxidation. DPV analysis revealed a linear detection range of 5–150 µM, with a detection limit (LOD) of 0.82 µM and a quantification limit (LOQ) of 2.48 µM. These results indicate that CeO2/NiO/GO is an effective and environmentally friendly material for the selective and sensitive detection of carbofuran in real samples. © 2025