Graphene oxide(GO) has received great interest for its unique properties and potential applications in separation.Here,(GO)@SiO2 composites-based stationary phase for high performance liquid chromatography(HPLC) were fabricated by covalently bonding GO onto aminosilica microspheres using N,N-dicyclohexylcarbodiimide as coupling agent.The reaction was achieved via coupling the amino groups of aminosilica and the carboxyl groups of GO.The prepared GO@SiO2 was characterized by scanning electron microscopy and Raman spectroscopy.GO@SiO2 composites were developed as stationary phase,and the chromatographic properties of bare SiO2 and GO@SiO2 were investigated by a series of polar compounds including melamine,cyanuric acid,clenbuterol,4-aminoantipyrine and 4-methylaminoantipyrine.Under the same conditions,GO@SiO2 column obtained a better separation for polar analytes in hydrophilic mode and the column was used as an analytical column for the determination of melamine in egg and milk samples.The proposed method was linear over the range of 0.2-50.0 μg/mL with a correlation coefficient(r) of 0.999 9.The limit of quantitation for melamine was 0.87 mg/kg.The recoveries of melamine at three spiked levels of 1,2,10 mg/kg ranged from 84.7% to 93.9% with relative standard deviations (RSDs) of 4.1%-6.3%.