The consumption of cereals and cereal products is expected to increase constantly along with the growth of world population. As staple food, cereals provide essential nutrients to the consumers. The most occurred problems associated to cereals and cereal products are mycotoxin outbreaks and adulteration. However, this sector is subject of several research works focused on the development of innovative formulation and analytical technique for quality control. For these reasons, quality control of cereal foods is a question of paramount importance. The available classical approach and technique (high-performance liquid chromatography, gas chromatography, enzyme-linked immunosorbent assays and physico-chemical analyses) for monitoring quality control present certain limitations and drawbacks in achieving the targeted objectives. These classical techniques are generally time consuming, destructive and require the use of sophisticated logistics for their implementation in the sector of cereal foods quality control. In addition, these classical analytical techniques suffer from disadvantages of destructiveness that may limit seriously their use for on-line monitoring, detection and evaluation. To face with the current challenges related to these issues, the use of rapid and nondestructive methods such as fluorescence spectroscopy is convenient and considered as the most potential among emerging technologies. Regarding fluorescence spectral data information, spectra provided excitation and emission wavelengths relevant to the presence of fluorophores in the cereal and cereal products. These outputs can be used as the most relevant indicators for setting quality control criteria. This chapter guides the quality control of cereal foods by using fluorescence spectroscopy and setting quality control criteria. The chapter includes information about fluorescence spectroscopy analysis related to different cereals and cereal products, i.e., flour, dough and bakery products, and details of chemical compositions, rheological properties, qualitative parameters, microbial spoilage and other contaminations as well as the authentication of cereal and cereal products.