Yerba mate is a beverage rich in bioactive compounds popular in South America. Polyphenols and methyl-xanthines were qualitatively and quantitatively analyzed in four commercial brands of yerba mate, as well as the antioxidant capacity of the beverages. Using LC/MSn analysis, 58 polyphenols were observed of which 4-sina-poylquinic acid, di-and tri-methoxycinnamoylquinic acids, two isomers of trimethoxycinnamoylshikimic acid and four isomers of caffeoyl-2,7-anhydro-3-deoxy-2-octulopyranosonic acid were identified for the first time in mate. Additionally, 46 polyphenols and 2 methylxanthines were quantified by HPLC-DAD. Hydroxycinnamic acid derivatives and flavonols comprised 90% and 10% of mate phenols, respectively, 3-caffeoylquinic (26.8-28.8%), 5-caffeoylquinic (21.1-22.4%), 4-caffeoylquinic (12.6-14.2%) and 3,5-dicaffeoylquinic acids (9.5-11.3%) along with rutin (7.1-7.8%) were the most abundant polyphenols, whereas caffeine was the main methylxanthine (90%). Ilex paraguariensis is an important source of polyphenols with moderate methylxanthines content; therefore its high antioxidant capacity was mainly associated to its polyphenolic composition.