A new analytical method was developed for the determination of melamine in milk powder by solid-phase extraction coupled with surface-enhanced Raman spectroscopy.The melamine in sample was extracted with acetonitrile,then adsorbed with activated carbon and eluted with sodium hydroxide solution.The results showed that the linear range for melamine was in the range of 0.005 0-1.6 mg/L,with a limit of detection of 0.100 mg/kg.While the method was applied in the analysis of melamine in milk powder,the recoveries for melamine were in the range of 75.3%-125%,and the relative standard deviations(n=5) were not more than 9.3%.With a remarkable effect in removing impurities,this method is accurate,reliable and sensitive in the rapid determination of melamine in milk powder,showing a great potential in monitoring the quality of milk powder.