The fluorescence spectroscopy is one of the method used to control the quality of food products through process and storage. Different modes of fluorescence spectra could be obtained on the food product: emission spectra, excitation spectra, synchronous spectra and excitation-emission spectra. In this chapter, the principle of fluorescence spectroscopy was illustrated as well as the fluorescence phenomena and instrumentation. The factors affecting the fluorescence signal are indicated. Finally, a briefly description of the fluorophores used in food and food products are presented.