This study investigated the effect of ultrasound-assisted extraction (UAE) and microwave-assisted extraction (MAE) conditions (extraction time, acetone concentration, solid-to-solvent ratio) on the efficiency of polyphenol recovery from distillery stillage and antioxidant activity of the extracts. The highest total polyphenol content, flavonoid content, and phenolic acid content were obtained with 10-min UAE and 5-min MAE at a solid-to-acetone ratio of 1:15 (w:v). Recovery yield was the highest with an aqueous solution of 60% acetone, confirming the results of Hansen Solubility Parameter analysis. Although UAE resulted in approximately 1.2 times higher extraction yield, MAE showed a better balance between extraction yield and energy consumption exhibited by its 3-fold higher extraction rate than that of UAE. Content of total polyphenols and phenolic acids strongly correlated with antioxidant activity, indicating that these compounds provide a substantial contribution to the bioactive properties of the extracts. Six phenolic acids were extracted, predominately ferulic and p-coumaric acids, and free forms of these acids constituted 91% of their total content, which opens various possibilities for their application in the food, cosmetics, and pharmaceutical industries.
Keywords: HPLC; bioactive compounds; distillery by-product; flavonoids; phenolic acids; waste valorization.