In this paper, capillary zone electrophoresis method was used for the determination of vitamin C and nicotinic acid content in black bean. 20 mmol/L borax solution and 20% acetonitrile concentration, 20kV voltage, 254 nm UV detection wavelength was chosen for electrophoretic analysis. Measured vitamin C and nicotinic acid content in black bean were 0.333 mg/g (RSD = 3.9%) (n = 5), 0.482 mg/g (RSD = 5.9%) (n = 5), respectively.