A highly sensitive nitrite (NO2−) electrochemical sensor is fabricated using glassy carbon electrode modified with Au nanoparticle and grapheme oxide. Briefly, this electrochemical sensor was prepared by drop-coating graphene oxide-chitosan mixed film on the surface of the electrode and then electrodepositing a layer of Au nanoparticle using cyclic voltammetry. The electrochemical behavior of NO2− on the sensor was investigated by cyclic voltammetry and amperometric i-t curve. The results showed that the sensor exhibited better electrocatalytic activity for NO2− in 0.1 mol/L phosphate buffer solution (PBS) (pH 5.0). The oxidation peak current was positively correlated with NO2− concentration in the ranges of 0.9 µM to 18.9 µM. The detection limit was estimated to be 0.3 µM. In addition, the interference of some common ions (e.g., NO3−, CO32−, SO42−, Cl−, Ca2+ and Mg2+) and oxidizable compound including sodium sulfite and ascorbic acid in the detection of nitrite was also studied. The results show that this sensor is more sensitive and selective to NO2−. Therefore, this electrochemical sensor provided an effective tool for the detection of NO2−.