The sensitive determination of VB(2)has broad analytical applications. In this work, a novel VB(2)electrochemical sensor based on the hydrothermal method was constructed to uniformly grow molybdenum disulfide and silver nanoparticles on the surface of electrospun carbon fiber. MoS2-Ag-CNF was characterized by scanning electron microscope, EDS spectrum, TEM analysis, cyclic voltammetry, differential pulse voltammetry, and electrochemical impedance spectroscopy. The sensor exhibited a high sensitivity of 0.05 to 40 mu M with a fast response time and a low detection limit of 0.02 mu M. The electrode also showed outstanding selectivity toward various interferences. These results indicate that the MoS2-Ag-CNF nanocomposites may be promising electrode materials for electrochemical biosensing.