The evaluation of volatiles in food is an important aspect of food production. It gives knowledge about the quality of foods and their relationship to consumers’ choices. Alcohols, aldehydes, acids, esters, terpenes, pyrazines, and furans are the main chemical groups that are involved in aroma formation. They are products of food processing: thermal treatment, fermentation, storage, etc. Food aroma is a mixture of varied molecules. Because of this, the analysis of aroma composition can be challenging. The four main steps can be distinguished in the evaluation of the volatiles in the food matrix as follows: (1) isolation and concentration; (2) separation; (3) identification; and (4) sensory characterization. The most commonly used techniques to separate a fraction of volatiles from non-volatiles are solid-phase micro-(SPME) and stir bar sorptive extractions (SBSE). However, to study the active components of food aroma by gas chromatography with olfactometry detector (GC-O), solvent-assisted flavor evaporation (SAFE) is used. The volatiles are mostly separated on GC systems (GC or comprehensive two-dimensional GCxGC) with the support of mass spectrometry (MS, MS/MS, ToF–MS) for chemical compound identification. Besides omics techniques, the promising part could be a study of aroma using electronic nose. Therefore, the main assumptions of volatolomics are here described.