Six kinds of samples are collected including pure milk, milk with high calcium and milk with high calcium but low fat producted by Inner Mongolia Yili Industrial Group Co.,Ltd.and Inner Mongolia Mengniu Dairy (Group) Co.,Ltd.respectively.0.17 mL, 0.20 mL, 0.23 mL, 0.26 mL, 0.29 mL, 0.32 mL, 0.35 mL of the six kinds of samples are added into 5mL deionized water, and 42 pieces of milk solution are obtained.Hitachi F-4600 fluorescence spectrophotometer is used to obtain the fluorescence spectra of the samples under excitation wavelength at 315 nm, 320 nm, 325 nm, 330 nm, 335 nm, 340 nm, 345 nm respectively.After Savitzky-Golay smoothing and FFT low-pass filtered, each fluorescence spectrum is decomposed by Gauss multi-dimensional fitting, then 5 element gauss peak appeared.Each element Gauss peak position of all milk peroxide solution is invariable under the same stimulation wave length.All element Gauss peaks are red shifted along with the stimulation wave length increasing.Under the long stimulation wave length, each element Gauss peak of milk with high calcium but low fat is bigger than the others.Milk density plays an unimportant role to the total fluorescence spectrum.