Biological, food, and water samples were used to determine the amount of Furazolidone (FUZ) in a variety of applications, including health and nutrition, diagnosis/treatment, pharmacological research, and food/drug quality monitoring. Using hydrothermal and ultrasonication strategies, new type of TiO2 (1D) and ZrO2 (0D) (TiO2/ZrO2) nanocomposites were prepared for FUZ determination. Then the prepared nanocomposite was characterization under X-ray diffraction, field emission scanning electron microscopy, high-resolution transmission electron microscopy, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, ultra violet visible spectroscopy, and the electrochemical property of the material was characterized by electrochemical impedance spectroscopy and cyclic voltammetry (CV). In addition, detection of FUZ was analyzed by electroanalytical studies such as CV and differential pulse voltammetry (DPV). This proposed TiO2/ZrO2/GCE sensor exhibits excellent electrochemical characteristics, including excellent linearity (0.01 – 537.22 µM), nanomolar detection limit (19 nM), and encouraging sensitivity (0.35 µA µM-1cm-2) and it shows greater selectivity, repeatability, and longer storage stability. Along with concerned realizability, the primed sensor was analyzed over biological samples that reveal good recovery in real samples.