In the present paper, the authors measured the fluorescences pectra of water, alcohols and major microcrystalline substances of different distilled spirits and synthesized their three-dimensional fluorescence spectra. By comparing the fluorescence spectra of major monomers with those of many different kinds of distilled spirits, the authors found that ethanol and many other monomers can influence the fluorescence spectra of distilled spirits. Apart from ethanol, the major microcrystalline substances, such as alcohols, acids, aldehydes and esters influence the fluorescences pectra of distilled spirits respectively. In the meanwhile, their influences are different. The influences of different kinds of monomers differ from each other in the respects of wavelength and intensity. The order of the influences from low level to high level is: alcohols, aldehydes, acids and esters. But the same kind of monomers can bring about almost the same fluorescence spectra. So, the same kind of monomers influences the fluorescence spectra of distilled spiritssimilarly. To sum up, the authors come to aconclusion that apart from water, every kind of monomers can influence the fluorescence spectra of distilled spirits. And the order of the influences from low level to high level is: alcohols, aldehydes, acids and esters. In the meanwhile, they in fluence the fluorescence spectra in different spectral range respectively. The outcome of the study is very important forthe further detailed research on the fluorescence spectra of distilled spirits in the future.