Olive pomace is a by-product of olive oil production that is toxic to the environment. The purpose of this study was to evaluate the methods of olive pomace valorization through the implementation of novel technology, the so-called microwave-assisted extraction process. To determine the total polyphenol content (TPC) and antioxidant activity (AA), polyphenol extraction using MAE was performed. Response surface methodology was used to determine the best extraction conditions, whereby the effects of three factors, solid ratio (g/50 mL), time (s), and power (W), were measured. The ferric reducing antioxidant power (FRAP) method was used to assess AA, whereas the spectrophotometric Folin–Ciocalteu (FC) method was used to determine TPC. The highest TPC of 15.30 mg of gallic acid equivalents per gram of dried weight (mg GAE/gdw) was generated after 105 s at 450 W, with a solid concentration of 1 g/50 mL, while the maximum AA was 10 mg of ascorbic acid equivalents per gram of dried weight (mg AAE/gdw). Numerical optimization revealed that 800 W, 180 s, and 1 g/50 mL were the best conditions for obtaining maximum TPC and AA.

With growing interest in sustainable solutions, olive pomace—a byproduct of olive oil production—has emerged as a source of bioactive compounds. This study investigates ultrasound-assisted extraction (UAE) as a green method for recovering antioxidant-rich polyphenols. A central composite design assessed the effects of extraction time (5–15 min), solid-to-solvent ratio (2–12 g per 100 mL), and ultrasound head size (small, medium, large) on total phenolic content (TPC) and antioxidant activity (AA). TPC ranged from 3.87 to 19.50 mg gallic acid equivalents per gram dry weight, while AA ranged from 3.31 to 11.15 mg ascorbic acid equivalents per gram dry weight. Solid-to-solvent ratio and head size had the strongest influence on TPC, with the large head at lower intensity producing the highest yield. The analysis revealed a positive link between TPC and AA ( r = 0.85, P < 0.001). UAE demonstrates efficiency and sustainability in valorizing olive pomace.