The potential impact of antibiotics in water environments affects aquatic organisms, microbial community structure, and resistance genes. In this work, we report the hydrothermal synthesis of twodimensional (2D) tungsten carbide (WC) nanoparticles on CO3 2- anion intercalated three-dimensional (3D) self-assembled nickel–cobalt layered double hydroxide (NiCo-LDH) nanorods, for the electrochemical determination of norfloxacin (NRF). The synergistic impact between the dual active components of the prepared electrode offered increased active surface area, high electrical conductivity, and prompt mass and ion diffusion, resulting in improved electrochemical performance for NRF monitoring. In ideal conditions, WC@NiCo-LDH modified electrode exhibited enhanced electrochemical characteristics, wide linear response (DPV = 0.02–83.4 lM and in i-t = 0.002–346 lM), and lowdetection limit (LOD) (DPV = 0. 005 lM and i-t = 0.002 lM). Furthermore, good reproducibility, virtuous operational and cycle stabilities, were obtained. The practical applications in real-world samples with acceptable recovery ranges were verified the interference-free sensing of NRF.