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This study utilized a simple hydrothermal method to synthesize nickel molybdenum oxide (NMO) for the detection of furazolidone (FZE). Our synthesized NMO was characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), field emission scanning electron spectroscopy (FE-SEM), and energy dispersive X-ray spectroscopy (EDX). The cyclic voltammetry (CV) and differential pulse voltammetry (DPV) were used to detect the FZE. Under optimized conditions, the obtained results showed that the NMO had an excellent electrocatalytic property towards FZE. As a result, NMO/GCE showed a good linear range of 0.001–1765 µM, an excellent detection limit (LOD) of 0.02 µM, and sensitivity of 0.2042 µA µM⁻¹ cm⁻².