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A method combining aqueous extraction, reversed-phase high-performance capillary liquid chromatography with photodiode array detection (cLC-DAD) and chemometric tools, was developed to determine phenolic compounds in residual brewing yeast. The effect of temperature, nature of extraction solvent and method for separation of extract solution were studied to optimize the extraction conditions on the basis of total phenolic content (TPC), total flavonoids content (TFC) and antioxidant capacity. Polyphenols were determined by cLC-DAD. Flavonols as rutin and kaempferol, flavonoids as naringin, phenolic acids as gallic acid and antioxidants as trans-ferulic and p-coumaric acids were found and quantified in the brewing residue. Data were subjected to evaluation using multifactor ANOVA and principal component analysis (PCA), both showing that lyophilization pretreatment affects the content of individual polyphenols and that residual brewing yeast contains higher polyphenol amounts than the liquid beer waste. The obtained results suggest that residual brewing yeast could be a source of polyphenols., Comunidad de Madrid Programa FEDER, Ministerio de Economía y Competitivad, Depto. de Química Analítica, Fac. de Ciencias Químicas, TRUE, pub