Food irradiation seems to be an effective and safe method for preventing microbial and insect contamination in cereals. Interestingly, the determination of the aroma-active compounds in irradiated and extruded rice flour does not yet exist. This study aimed to investigate aroma and aroma-active compounds of non-irradiated rice flour (NIRF) and irradiated and processed rice flour (IPRF) by the SPME method combined with GC-MS-O. In the present study, twenty-three aroma-active compounds in the NIRF sample while fifteen in the IPRF sample were identified with 1.6–4.9 odor intensity scores. Hexanal [4.9], nonanal [4.4], heptanal [3.9], decanal [3.3], 3-Octen-2-one [3.1] and were detected as key odorants in all samples. Whereas, 2-penthylfuran [3.8], octanal [3.8], nonanal [4.5], and benzaldehyde [2.1] were clearly higher in the IPRF sample, considering NIRF. The amount of hexanal which can be considered as irradiation odor (IO), has been increased due to the food irradiation process.