Abstract:Mezcal is a traditional Mexican spirit produced by distilling fermented Agave. The effects of Agave species, origin, and season on the volatile compound profile were studied in mezcal from Oaxaca, Mexico. Liquid-liquid extraction was used to isolate volatile compounds from mezcals made from Agave angustifolia Haw. and Agave potatorum Zucc. These compounds were identified using gas chromatography-mass spectrometry (GC-MS). Eighty-four volatile compounds were identified, including alcohols, esters, fatty acids, ketones, furans, and others. Using variance analysis, it was possible to observe significant differences for the 26, 24, and 10 compounds in mezcal samples that differed based on Agave species, origin, and season. 3-Ethyl-phenol was identified only in samples of mezcal from A. angustifolia, and this volatile compound could be used as an authentic marker of mezcal from A. angustifolia (p ≤ 0.01).