Developing a precise and effective method to detect Nilutamide (NIL) is essential due to its contamination of the environment, which poses significant risks to human health and the biosphere. In this study, we employed a simple hydrothermal technique to create a nanocomposite of CuCo2O4 (copper cobalt oxide) and multi-walled carbon nanotube (MWCNT), which was then anchored onto a glassy carbon electrode for NIL detection. Various spectroscopic techniques were employed to confirm the structure of the nanomaterial, and its electrochemical properties were examined using cyclic voltammetry, differential pulse voltammetry, and electrochemical impedance spectroscopy. The CuCo2O4/MWCNT nanocomposite-modified electrode exhibited a wide linear detection range from 0.01 to 170 µM, a high sensitivity of 1.50 μA μM−1 cm−2, a low detection limit of 0.01 μM, outstanding stability, repeatability, and practical applicability for NIL detection.