An HPLC-MS/MS method was developed for the determination of acid orange Ⅱ and metanil yellow in food such as bean products,vegetables,pepper products,hotpot condiment,meat and aquatic products.The samples were extracted with 70% acetonitrile.The crude extracts were further purified with an Oasis WAX SPE column,and then filtered through a polytetrafluoroethylene(PTFE) organic membrane.The separation was performed on a Thermo Hypersil Gold aQ(100 mm×2.1 mm,1.9 μm) column by gradient elution using acetonitrile-water as mobile phase.The analytes were analyzed in electrospray ionization(ESI-) under multi reaction monitoring(MRM) mode,and quantified by the matrix matched external standard method.The results showed that the acid orange Ⅱ and metanil yellow in the six samples displayed good peak shapes.The calibration curves were linear in the range of 1.0- 20 μg?L-1,with correlation coefficients more than 0.995.The quantitation limits(LOQ,S/N=10) of acid orange Ⅱ and metanil yellow in low-fat food products(bean-products,vegetables and pepper products) were 1.4,1.0 μg?kg-1,respectively,and in high-fat foods(hotpot condiment,meat and aquatic products) were 2.0,1.4 μg?kg-1,respectively.The recoveries of acid orange Ⅱ and metanil yellow in the six samples were in the range of 65.8%-99.0% with relative standard deviations (RSD) of 2.4% - 6.0%.The method was sensitive and reliable in the determination of acid orange Ⅱ and metanil yellow in food products.