We have described a hybrid material that consists of molybdenum disulfide nanosheets (MoS2) coated on functionalized multiwalled carbon nanotubes (f-MWCNTs) for sensitive and selective determination of chloramphenicol (CAP). The MoS2/f-MWCNTs nanocomposite was successfully prepared through a hydrothermal process and its structure was characterized by scanning electron microscopy, transmission electron microscopy, energy-dispersive X-ray spectroscopy, electrochemical impedance spectroscopy and cyclic voltammetry. The MoS2/f-MWCNTs nanocomposite holds excellent electrochemical properties and it displays excellent electrocatalytic ability to CAP. Under optimized working conditions, the nanocomposite film modified electrode responds linearly to CAP in the concentration range of 0.08–1392 μM. The detection limit was obtained as 0.015 μM (±0.003). The electrode has high level of selectivity in presence of large excess concentrations of interfering species. In addition, the modified electrode offers satisfactory repeatability, reproducibility and stability. The practical applicability of the electrode was demonstrated in food samples such as, milk, powdered milk and honey samples and the recoveries are agreeable which clearly revealed its practical feasibility in food analysis.