A series of CuFe2O4 nanoparticles was synthesized with the assistance of organic amines or inorganic bases via a hydrothermal method. The prepared samples were confirmed as a spinel-type structure by x-ray diffraction. The shapes of the samples were detected by transmission electron microscope (TEM), which confirmed that all the synthesized samples were nanoparticles. The electrocatalytic properties of the samples modified on a glassy carbon electrode were investigated for the reduction of p-nitrophenol, potassium chromate (K2CrO4), and sodium nitrite (NaNO2) in basic solution using the cyclic voltammetry method. The results showed that all the samples showed enhanced catalytic activity for the reduction of p-nitrophenol, K2CrO4, and NaNO2. Among the samples, CuFe2O4 prepared with cyclohexylamine (S-2) showed the highest catalytic activity for p-nitrophenol reduction, whereas CuFe2O4 prepared with NaOH and PVP (S-4) showed the highest activity for both K2CrO4 and NaNO2 reduction in basic solution.