ABSTRACT.- Solid Phase Microextraction or SPME was created to facilitate faster sample preparation, both in the laboratory and wherever the sampling site is located. Solid phase microextraction (SPME) was developed by Pawliszyn's group in 1990 as a solvent-free technique on the basis of adsorption-absorption theory. SPME is based on the principle that analytes are distributed between the sample matrix and the fiber coating. The fiber is built of fused silica and covered with a sorbent (polymeric materials identical to those used as stationary phase in gas chromatography columns). The transport of the analytes from the sample matrix to the fiber begins when the fiber comes into contact with the sample. The analytes are then desorbed by temperature or with an organic solvent. The extraction is complete and satisfactory when the analyte has reached an equilibrium concentration of distribution between the sample and the fiber. Even being experimentally a non-exhaustive extractive technique (it is an equilibrium), SPME has been rapidly adopted as a simple, miniaturized, and green technique, which combines sampling, extraction, concentration, cleanup and sample introduction in a single step. These characteristics transformed SPME in one of the most used techniques for different applications related to analytical chemistry. In this chapter, we will present different number of examples by which SPME focuses in the characterization of both food aroma and frequent odor defects.. © 2023 American Chemical Society. All rights reserved.