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The use of guayusa (Ilex guayusa Loes.) leaves as functional food has increase recently. This work discusses the antioxidant activity and volatile compounds of guayusa leaves extract and fractions. The methanol crude extract was obtained by maceration, subsequently hexane, chloroform, ethyl acetate, and aqueous fractions were collected by solvent-solvent partition. Total phenolic content (TPC), total flavonol/flavone content (TFC), 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging activity, and ferric reducing antioxidant power (FR