Abstract: The ZnSn(OH)₆ microspheres were prepared by one-step hydrothermal method, which were compounded with two-dimensional Ti₃C₂ MXene nanosheets to obtain ZnSn(OH)₆/Ti₃C₂ MXene nanocomposite, and a novel electrochemical sensor was fabricated based on this material. The irreversible oxidation peak of nitrofurazone was firstly studied on this sensor by using cyclic voltammetry. The voltammetric process of nitrofurazone was adsorption-controlled and the electron transfer number of this oxidation reaction was 2. The differential pulse voltammetry was used for the quantitative analysis of nitrofurazone, and the results showed that this sensor had remarkable catalytic effect for the electrochemical oxidation of nitrofurazone owing to the synergistic effect of ZnSn(OH)₆ microspheres and two-dimensional Ti₃C₂ MXene. The concentration of nitrofurazone had good linear relationship with its oxidation peak current in the range of 0.5~70 μmol/L.The detection limit was 0.16 μmol/L (R_SN=3). The sensor displayed excellent repeatability for the detection of nitrofurazone, exhibiting a relative standard derivation (RSD) (n=10) of 3.4%. This sensing platform was applied to the analysis of animal-derived foods with the recovery ranging between 92.0% and 107%.