The interaction of dibazol to serum was investigated by fluorescence and UV-vis spectroscopy. The fluorescence experiment results show that the fluorescence of human serum can be effectively induced by light wave. The maximum fluorescence intensity of serum is excited at 280 nm and the peak wavelength is about 334 nm. It can also be concluded that the fluorescence intensity gradually increase with the increasing excitation light wavelength. The range of the fluorescence spectroscopy of serum-dibazol system induced by excited at different wavelength is about 290 - 450 nm. The fluorescence intensity of the interaction system of dibazol-serum is significantly reduced, indicating that the fluorescence quenching of serum occurred strongly caused by dibazol and there is a new compound formed between dibazol and serum. The absorption spectra show that there is a large blue in the system of dibazol and serum, which reveal that there is a kind of new complex between dibazol and serum. It is very significance to study the interaction between dibazol and serum for understanding of drug’s toxicity and its distribution in the organism.