A method for the simultaneous determination of red 2G, dimethyl yellow and diethyl yellow in meat products, soybean products and flavoring was established by HPLC and LC-MS. The samples were extracted by acetonitrile aqueous solution, with solid phase column, and determined by HPLC with diode array detector or UV detector, and then quantified by external standard method. The detection limit of red 2G was 0.5 mg/kg, and those of dimethyl yellow and diethyl yellow were 0.1 mg/kg, with the recovery rate ranging from 80.7% to 91.8% and the relative standard deviation of 3.8%~7.8%.