By using a three-electrode setup consisting of a working electrode made up of glassy carbon, a counter electrode made up of platinum, and a reference electrode made up of saturated calomel, the cyclic voltammetry was utilized to measure the content of tartrazine and sunset yellow FCF in five goods sold in the market and the measurement method was optimized. The result indicated by the cyclic voltammetry curve that the peak current was linearly correlated to the analyte concentration within the range of 0.1~0.8 μg/mL. The concentration of tartrazine and sunset yellow FCF in the five samples were measured to be respectively in the range of 4.88~6.06 mg/kg and 4.37~5.22 mg/kg, which were both lower than the national standards. The Method Detection Limit (MDL) of this measurement of the concentration of tartrazine and sunset yellow FCF was 1.12 mg/kg and 1.43 mg/kg respectively. Their relative standard deviations of the test results for lemon yellow and sunset yellow were 2.1% and 2.3% (n=6). With satisfying accuracy, this approach featureed a recovery rate of the target component ranging from 91.5% and 114.5% when the fortified level was 2.0 mg/kg.