A C60modified carbon paste electrode(MCPE) was prepared and its electrochemical properties in tetrabutylammonium hydroxide/CH3CN/H2O solutions were studied. Two pairs of mono-electron quasi-reversible redox peaks were obtained and characterized. The experimental results revealed that this electrode had a good electrocatalytic reduction response for nitrobenzene in these conditions. The catalytic reduction current had a good linear relationship to the concentration of nitrobenzene. The linear range of nitrobenzene concentration was between 5.0×10−5∼6.0×10−3mol/L. The detection limit was 3.0×10−5mol/L.