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Different extraction techniques were used to exploit fruit processing residues for their use as a source of phenolic compounds. Three different extraction methods, namely microwave-assisted extraction (MAE), subcritical water extraction (SWE), and maceration (M), were assessed to gauge their respective efficacies. Total phenolic content (TPC) and total flavonoid content (TFC), ferric reducing antioxidant power (FRAP), and radical scavenging activity ABTS assay were evaluated. High-performance liquid chromatography was used to assess the polyphenolic profile. MAE was the extraction technique that allowed the highest recovery of polyphenolic compounds. Concerning the fruit by-products analyzed, the extract of pomegranate peels obtained using M60C and MAE had the highest TPC (313 ± 24 mg GAE/g dry weight (dw)) and TFC (36.0 ± 2.8 mg EE/g dw), respectively, and the highest antioxidant activity (FRAP = 740 ± 67 mg AAE/g dw and ABTS (628 ± 27 mg TE/g dw) corresponded to M60C. The phenolic composition obtained for this sample using high-performance liquid chromatographic–diode array detection (HPLC–DAD) showed that gallic acid, protocatechuic acid, β-resorcylic acid, (+)-cathechin, and rutin were the main phenolics found. The findings underscore the capacity of agricultural by-products to act as a source of phenolic compounds. This offers a feasible solution to enhance the nutritional content in food while simultaneously minimizing environmental waste.