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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 \u00b1 24 mg GAE\/g dry weight (dw)) and TFC (36.0 \u00b1 2.8 mg EE\/g dw), respectively, and the highest antioxidant activity (FRAP = 740 \u00b1 67 mg AAE\/g dw and ABTS (628 \u00b1 27 mg TE\/g dw) corresponded to M60C. The phenolic composition obtained for this sample using high-performance liquid chromatographic\u2013diode array detection (HPLC\u2013DAD) showed that gallic acid, protocatechuic acid, \u03b2-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.<\/jats:p>","DOI":"10.3390\/pr11061767","type":"journal-article","created":{"date-parts":[[2023,6,12]],"date-time":"2023-06-12T01:28:21Z","timestamp":1686533301000},"page":"1767","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":13,"title":["A Critical Assessment of Extraction Methodologies for the Valorization of Agricultural Wastes: Polyphenolic Profile and Bioactivity"],"prefix":"10.3390","volume":"11","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-0924-9681","authenticated-orcid":false,"given":"Cristina","family":"Soares","sequence":"first","affiliation":[{"name":"REQUIMTE\/LAQV, Instituto Superior de Engenharia do Porto, Instituto Polit\u00e9cnico do Porto, Rua Dr. Ant\u00f3nio Bernardino de Almeida 431, 4249-015 Porto, Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1500-9211","authenticated-orcid":false,"given":"Manuela M.","family":"Moreira","sequence":"additional","affiliation":[{"name":"REQUIMTE\/LAQV, Instituto Superior de Engenharia do Porto, Instituto Polit\u00e9cnico do Porto, Rua Dr. Ant\u00f3nio Bernardino de Almeida 431, 4249-015 Porto, Portugal"}]},{"given":"Sandra","family":"Ramos","sequence":"additional","affiliation":[{"name":"Laborat\u00f3rio de Engenharia Matem\u00e1tica, Instituto Superior de Engenharia do Porto\u2014Instituto Polit\u00e9cnico do Porto, Rua Dr. Ant\u00f3nio Bernardino de Almeida 431, 4249-015 Porto, Portugal"},{"name":"Centro de Estat\u00edstica e Aplica\u00e7\u00f5es da Universidade de Lisboa, Faculdade de Ci\u00eancias da Universidade de Lisboa, Bloco C6-Piso 4, 1749-016 Lisboa, Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-1951-3557","authenticated-orcid":false,"given":"M. J.","family":"Ramalhosa","sequence":"additional","affiliation":[{"name":"REQUIMTE\/LAQV, Instituto Superior de Engenharia do Porto, Instituto Polit\u00e9cnico do Porto, Rua Dr. Ant\u00f3nio Bernardino de Almeida 431, 4249-015 Porto, Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-3014-5089","authenticated-orcid":false,"given":"Manuela","family":"Correia","sequence":"additional","affiliation":[{"name":"REQUIMTE\/LAQV, Instituto Superior de Engenharia do Porto, Instituto Polit\u00e9cnico do Porto, Rua Dr. Ant\u00f3nio Bernardino de Almeida 431, 4249-015 Porto, Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-1559-4492","authenticated-orcid":false,"given":"Jaroslava","family":"Svarc-Gaji\u0107","sequence":"additional","affiliation":[{"name":"Faculty of Technology, University of Novi Sad, Bulevar cara Lazara 1, 21000 Novi Sad, Serbia"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-3924-776X","authenticated-orcid":false,"given":"Cristina","family":"Delerue-Matos","sequence":"additional","affiliation":[{"name":"REQUIMTE\/LAQV, Instituto Superior de Engenharia do Porto, Instituto Polit\u00e9cnico do Porto, Rua Dr. Ant\u00f3nio Bernardino de Almeida 431, 4249-015 Porto, Portugal"}]},{"given":"M. F\u00e1tima","family":"Barroso","sequence":"additional","affiliation":[{"name":"REQUIMTE\/LAQV, Instituto Superior de Engenharia do Porto, Instituto Polit\u00e9cnico do Porto, Rua Dr. Ant\u00f3nio Bernardino de Almeida 431, 4249-015 Porto, Portugal"}]}],"member":"1968","published-online":{"date-parts":[[2023,6,10]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","first-page":"93","DOI":"10.1016\/j.gfs.2019.01.002","article-title":"Food Waste Accounting Methodologies: Challenges, Opportunities, and Further Advancements","volume":"20","author":"Corrado","year":"2019","journal-title":"Glob. Food Secur."},{"key":"ref_2","unstructured":"(2022, November 24). Food and Agriculture Organization of the United Nations (FAO) Overview|Sustainable Development Goals|Food and Agriculture Organization of the United Nations. 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