In this study, we developed an excellent electrocatalyst of NiMoO4 doped with CdO and then coated electrochemical detection of chloramphenicol (CAP) via a glassy carbon electrode (NiMoO4@CdO/GCE). In particular, this drug treats typhoid, fever, and salmonellosis infections. CAP detection and measurements have become progressively important in ensuring human safety. The NiMoO4@CdO nanocomposite was prepared using the one-step hydrothermal method and characterized for its structural and optical properties. The electrochemical determination of CAP was investigated using cyclic voltammetry (CV), differential pulse voltammetry (DPV), and electrochemical impedance spectroscopy (EIS) techniques. We observed that the glassy carbon electrode modified with NiMoO4@CdO efficiently reduced the CAP at a very low potential. While CAP interacts with this system, metal oxide nanocomposites can combine with CAP reduction to produce phenylhydroxylamine. According to the DPV analysis, the bare electrode provides a linear response in the 10–100 µM range and a substantial reduction in CAP over a low detection limit of 0.083 µM when compared to (NiMoO4@CdO/GCE). Other co-existing molecules challenge the utility of this sensor. Additionally, this sensor exhibited high selectivity, stability, and reproducibility. Further, we evaluated the sensor for real-sample analysis, and the results were satisfactory.