Melamine is a kind of triazine compound and the fluorescence of it can get enhanced in the presence of cationic surfactant in weak alkaline medium. A new fluorescent spectrophotometry based on this principle) has been developed to determine melamine under the optimum conditions such as Tris-HCl buffersolution), pH 8.0 and with CTMAB as sensitizing agent. The linear range, detection limit and relative standard deviation were 25-1000 μg/L, 19 μg/L and 1.6%,respectively. The samples were pretreated according to the solid phase extraction monolithic column to carry out the detection of real milk. This method is simple, rapid and accurate. It can be used to screen and detect the milk samples primarily.