{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,5,27]],"date-time":"2026-05-27T21:24:42Z","timestamp":1779917082709,"version":"3.53.1"},"reference-count":47,"publisher":"MDPI AG","issue":"6","license":[{"start":{"date-parts":[[2025,6,3]],"date-time":"2025-06-03T00:00:00Z","timestamp":1748908800000},"content-version":"vor","delay-in-days":0,"URL":"https:\/\/creativecommons.org\/licenses\/by\/4.0\/"}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Antioxidants"],"abstract":"<jats:p>Selecting factors that significantly affect the extraction process and optimizing them are essential to obtain high extraction efficiency. This study aimed at optimizing the ultrasonic-assisted extraction (UAE) of polyphenols from Romanian blackthorn fruits using aqueous solutions of ethanol as green extraction solvents. Six process factors, including solvent\/plant material ratio (RLS = 4.95\u201315.1 cm3\/g), ethanol concentration in the extraction solvent (cet = 16.4\u201383.6%), extraction temperature (t = 30\u201370 \u00b0C), pH of the solvent (pH = 2\u20137), amplitude of the ultrasonic probe (A = 30\u201370%), and extraction time (\u03c4 = 5\u201315 min), were screened and optimized based on a Plackett\u2013Burman design (PBD) and a central composite design (CCD). Statistical analysis indicated that RLS, cet, and t significantly affected the process response variables in terms of total phenolic content (TPC), total anthocyanin content (TAC), and antioxidant capacity (AC). Under optimal conditions (RLS,opt = 15.1 cm3\/g, cet,opt = 33.2%, topt = 66.8 \u00b0C, pHopt = 7, Aopt = 50%, and \u03c4opt = 10 min), the following levels of response variables were experimentally determined: TPCopt = 14.45 \u00b1 0.718 mg GAE\/g DM, TACopt = 0.405 \u00b1 0.057 mg C3GE\/g DM, and ACopt = 16.75 \u00b1 1.144 mg TE\/g DM. Six phenolic compounds were identified in the extract obtained at optimal levels of process factors, i.e., rutin (7.12 \u00b1 0.06 mg\/100 g DM), protocatechuic acid (6.83 \u00b1 0.01 mg\/100 g DM), neochlorogenic acid (4.88 \u00b1 0.01 mg\/100 g DM), vanillic acid (3.70 \u00b1 0.01 mg\/100 g DM), chlorogenic acid (1.93 \u00b1 0.02 mg\/100 g DM), and caffeic acid (1.51 \u00b1 0.01 mg\/100 g DM).<\/jats:p>","DOI":"10.3390\/antiox14060680","type":"journal-article","created":{"date-parts":[[2025,6,3]],"date-time":"2025-06-03T06:21:51Z","timestamp":1748931711000},"page":"680","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":11,"title":["Optimization of Ultrasound-Assisted Extraction of Phenolic Compounds from Romanian Blackthorn (Prunus spinosa L.) Fruits"],"prefix":"10.3390","volume":"14","author":[{"given":"Ana-Maria","family":"Dr\u0103ghici-Popa","sequence":"first","affiliation":[{"name":"Department of Organic Chemistry, National University of Science and Technology POLITEHNICA Bucharest, 1-7 Gheorghe Polizu St., 011061 Bucharest, Romania"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-1747-9930","authenticated-orcid":false,"given":"Oana Cristina","family":"P\u00e2rvulescu","sequence":"additional","affiliation":[{"name":"Department of Chemical and Biochemical Engineering, National University of Science and Technology POLITEHNICA Bucharest, 1-7 Gheorghe Polizu St., 011061 Bucharest, Romania"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Raluca","family":"Stan","sequence":"additional","affiliation":[{"name":"Department of Organic Chemistry, National University of Science and Technology POLITEHNICA Bucharest, 1-7 Gheorghe Polizu St., 011061 Bucharest, Romania"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-4373-295X","authenticated-orcid":false,"given":"Ana-Maria","family":"Brezoiu","sequence":"additional","affiliation":[{"name":"Department of Chemical and Biochemical Engineering, National University of Science and Technology POLITEHNICA Bucharest, 1-7 Gheorghe Polizu St., 011061 Bucharest, Romania"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"1968","published-online":{"date-parts":[[2025,6,3]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","unstructured":"Gonz\u00e1lez-de-Peredo, A.V., V\u00e1zquez-Espinosa, M., Espada-Bellido, E., Ferreiro-Gonz\u00e1lez, M., Carrera, C., Palma, M., \u00c1lvarez, J.A., Barbero, G.F., and Ayuso, J. (2020). Optimization of analytical ultrasound-assisted methods for the extraction of total phenolic compounds and anthocyanins from sloes (Prunus spinosa L.). Agronomy, 10.","DOI":"10.3390\/agronomy10070966"},{"key":"ref_2","doi-asserted-by":"crossref","first-page":"2625","DOI":"10.1007\/s13738-021-02217-9","article-title":"Optimization of extraction conditions of polyphenols, antioxidant capacity and sun protection factor from Prunus spinosa fruits. Application in sunscreen formulation","volume":"18","author":"Soran","year":"2021","journal-title":"J. Iran. Chem. Soc."},{"key":"ref_3","doi-asserted-by":"crossref","first-page":"125373","DOI":"10.1016\/j.foodchem.2019.125373","article-title":"Comparison between polyphenol profile and bioactive response in blackthorn (Prunus spinosa L.) genotypes from north Serbia-from raw data to PCA analysis","volume":"302","author":"Duarte","year":"2020","journal-title":"Food Chem."},{"key":"ref_4","doi-asserted-by":"crossref","first-page":"346","DOI":"10.1007\/s10600-015-1278-8","article-title":"Phenolic components and antioxidant activity of Prunus spinosa from Gumushane, Turkey","volume":"51","author":"Aliyazicioglu","year":"2015","journal-title":"Chem. Nat. Compd."},{"key":"ref_5","first-page":"90","article-title":"Determination of chemical composition and fatty acids of blackthorn fruits (Prunus spinosa) grown near Cluj-Napoca, NW Romania","volume":"105","author":"Grebla","year":"2018","journal-title":"Agricultura"},{"key":"ref_6","doi-asserted-by":"crossref","first-page":"247","DOI":"10.1016\/j.foodchem.2009.10.016","article-title":"Strawberry-tree, blackthorn and rose fruits: Detailed characterisation in nutrients and phytochemicals with antioxidant properties","volume":"120","author":"Barros","year":"2010","journal-title":"Food Chem."},{"key":"ref_7","doi-asserted-by":"crossref","first-page":"6571","DOI":"10.1021\/jf300873k","article-title":"New beverages of lemon juice enriched with the exotic berries maqui, a\u00e7a\u0131, and blackthorn: Bioactive components and in vitro biological properties","volume":"60","author":"Moreno","year":"2012","journal-title":"J. Agric. Food Chem."},{"key":"ref_8","doi-asserted-by":"crossref","unstructured":"Oancea, A.G., Saracila, M., Vlaicu, P.A., Varzaru, I., Untea, A.E., and Dragomir, C. (2024). Assessment of the antioxidant potential of blackthorns and hawthorns: Comparative analysis and potential use in ruminants\u2019 nutrition. Separations, 11.","DOI":"10.3390\/separations11090275"},{"key":"ref_9","doi-asserted-by":"crossref","first-page":"100079","DOI":"10.1016\/j.meafoo.2023.100079","article-title":"Quality attributes and antioxidant activity of three wild plums from Prunus spinosa and Prunus domestica species","volume":"10","author":"Ozzengin","year":"2023","journal-title":"Meas Food"},{"key":"ref_10","doi-asserted-by":"crossref","first-page":"49","DOI":"10.1016\/j.jff.2015.09.015","article-title":"Phenolic compounds of blackthorn (Prunus spinosa L.) and influence of in vitro digestion on their antioxidant capacity","volume":"19","author":"Pinacho","year":"2015","journal-title":"J. Funct. Foods"},{"key":"ref_11","doi-asserted-by":"crossref","first-page":"61","DOI":"10.1051\/fruits\/2013102","article-title":"Wild blackthorn (Prunus spinosa L.) and hawthorn (Crataegus monogyna Jacq.) fruits as valuable sources of antioxidants","volume":"69","year":"2014","journal-title":"Fruits"},{"key":"ref_12","doi-asserted-by":"crossref","first-page":"297","DOI":"10.2298\/HEMIND130312054V","article-title":"Phenolic composition, antioxidant and antimicrobial activity of the extracts from Prunus spinosa L. fruit","volume":"68","year":"2014","journal-title":"Hem. Ind."},{"key":"ref_13","doi-asserted-by":"crossref","first-page":"105","DOI":"10.2298\/ABS191217004V","article-title":"Examination of the polyphenol content and bioactivities of Prunus spinosa L. fruit extracts","volume":"72","author":"Ivanov","year":"2020","journal-title":"Arch. Biol. Sci."},{"key":"ref_14","doi-asserted-by":"crossref","unstructured":"Kotsou, K., Stoikou, M., Athanasiadis, V., Chatzimitakos, T., Mantiniotou, M., Sfougaris, A.I., and Lalas, S.I. (2023). Enhancing antioxidant properties of Prunus spinosa fruit extracts via extraction optimization. Horticulturae, 9.","DOI":"10.3390\/horticulturae9080942"},{"key":"ref_15","doi-asserted-by":"crossref","unstructured":"Magiera, A., Czerwi\u0144ska, M.E., Owczarek, A., Marchelak, A., Granica, S., and Olszewska, M.A. (2022). Polyphenol-enriched extracts of Prunus spinosa fruits: Anti-inflammatory and antioxidant effects in human immune cells ex vivo in relation to phytochemical profile. Molecules, 27.","DOI":"10.3390\/molecules27051691"},{"key":"ref_16","doi-asserted-by":"crossref","unstructured":"Mar\u010deti\u0107, M., Samard\u017ei\u0107, S., Ili\u0107, T., Bo\u017ei\u0107, D.D., and Vidovi\u0107, B. (2022). Phenolic composition, antioxidant, anti-enzymatic, antimicrobial and prebiotic properties of Prunus spinosa L. fruits. Foods, 11.","DOI":"10.3390\/foods11203289"},{"key":"ref_17","doi-asserted-by":"crossref","first-page":"469","DOI":"10.1007\/s00217-018-3178-1","article-title":"Nutraceutical properties and phytochemical characterization of wild Serbian fruits","volume":"245","author":"Bosco","year":"2019","journal-title":"Eur. Food Res. Technol."},{"key":"ref_18","first-page":"813","article-title":"Antioxidant and antimicrobial activity of polyphenol extracts from wild berry fruits grown in southeast Serbia","volume":"12","year":"2013","journal-title":"Trop. J. Pharm. Res."},{"key":"ref_19","doi-asserted-by":"crossref","first-page":"507","DOI":"10.1556\/1326.2017.00327","article-title":"Determination of phenolic compounds, antioxidant capacity and organic acids contents of Prunus domestica L., Prunus cerasifera Ehrh. and Prunus spinosa L. fruits by HPLC","volume":"29","author":"Celik","year":"2017","journal-title":"Acta Chromatogr."},{"key":"ref_20","first-page":"3643","article-title":"In-Vitro antioxidant and antimicrobial activity of aerial parts of Prunus spinosa L. growing wild in Bosnia and Herzegovina","volume":"12","year":"2021","journal-title":"Int. J. Pharm. Sci. Res."},{"key":"ref_21","doi-asserted-by":"crossref","unstructured":"Negrean, O.R., Farcas, A.C., Pop, O.L., and Socaci, S.A. (2023). Blackthorn\u2014A valuable source of phenolic antioxidants with potential health benefits. Molecules, 28.","DOI":"10.3390\/molecules28083456"},{"key":"ref_22","doi-asserted-by":"crossref","unstructured":"Olszewska, M.A., Zimi\u0144ska, A., Draszanowska, A., and Sawicki, T. (2024). Blackthorn fruit peel polyphenol extracts and photodynamic effect under blue light against Listeria monocytogenes. Food Microbiol., 124.","DOI":"10.1016\/j.fm.2024.104608"},{"key":"ref_23","doi-asserted-by":"crossref","unstructured":"Tiboni, M., Coppari, S., Casettari, L., Guescini, M., Colomba, M., Fraternale, D., Gorassini, A., Verardo, G., Ramakrishna, S., and Guidi, L. (2020). Prunus spinosa extract loaded in biomimetic nanoparticles evokes in vitro anti-inflammatory and wound healing activities. Nanomaterials, 11.","DOI":"10.3390\/nano11010036"},{"key":"ref_24","doi-asserted-by":"crossref","first-page":"540","DOI":"10.1016\/j.ultsonch.2016.06.035","article-title":"Ultrasound assisted extraction of food and natural products. Mechanisms, techniques, combinations, protocols and applications. A review","volume":"34","author":"Chemat","year":"2017","journal-title":"Ultrason. Sonochem."},{"key":"ref_25","doi-asserted-by":"crossref","first-page":"1135","DOI":"10.18203\/2319-2003.ijbcp20202566","article-title":"Herbal extraction procedures: Need of the hour","volume":"9","author":"Saravanabavan","year":"2020","journal-title":"Int. J. Basic Clin. Pharmacol."},{"key":"ref_26","doi-asserted-by":"crossref","unstructured":"Gavrila, A.I., Damian, E.J., Rosca, A., Calinescu, I., Hodosan, C., and Popa, I. (2025). Optimization of microwave-assisted extraction of polyphenols from Crataegus monogyna L. Antioxidants, 14.","DOI":"10.3390\/antiox14030357"},{"key":"ref_27","doi-asserted-by":"crossref","unstructured":"Gavrila, A.I., Zalaru, C.M., Tatia, R., Seciu-Grama, A.M., Negrea, C.L., Calinescu, I., Chipurici, P., Trifan, A., and Popa, I. (2023). Green extraction techniques of phytochemicals from Hedera helix L. and in vitro characterization of the extracts. Plants, 12.","DOI":"10.20944\/preprints202311.0492.v1"},{"key":"ref_28","doi-asserted-by":"crossref","unstructured":"Naoum, E., Xynopoulou, A., Kotsou, K., Chatzimitakos, T., Athanasiadis, V., Bozinou, E., and Lalas, S.I. (2024). The value of using green extraction techniques to enhance polyphenol content and antioxidant activity in Nasturtium officinale leaves. Appl. Sci., 14.","DOI":"10.3390\/app142210739"},{"key":"ref_29","doi-asserted-by":"crossref","unstructured":"Oro, C.E.D., Wancura, J.H., Santos, M.S.D., Venquiaruto, L.D., Dallago, R.M., and Tres, M.V. (2025). High-pressure extraction techniques for efficient recovery of flavonoids and coumarins from flower seeds. Processes, 13.","DOI":"10.3390\/pr13020300"},{"key":"ref_30","doi-asserted-by":"crossref","first-page":"106646","DOI":"10.1016\/j.ultsonch.2023.106646","article-title":"A comprehensive review of ultrasonic assisted extraction (UAE) for bioactive components: Principles, advantages, equipment, and combined technologies","volume":"101","author":"Shen","year":"2023","journal-title":"Ultrason. Sonochem."},{"key":"ref_31","doi-asserted-by":"crossref","unstructured":"Vilas-Boas, A.A., Gomez-Garcia, R., Machado, M., Nunes, C., Ribeiro, S., Nunes, J., Oliveira, A.L.S., and Pintado, M. (2023). Lavandula pedunculata polyphenol-rich extracts obtained by conventional, MAE and UAE methods: Exploring the bioactive potential and safety for use a medicine plant as food and nutraceutical ingredient. Foods, 12.","DOI":"10.3390\/foods12244462"},{"key":"ref_32","doi-asserted-by":"crossref","first-page":"131550","DOI":"10.1016\/j.seppur.2025.131550","article-title":"Molecular simulation and machine learning assisted in exploring betaine-based deep eutectic solvent extraction of active compounds from peony petals","volume":"361","author":"Wang","year":"2025","journal-title":"Sep. Purif. Technol."},{"key":"ref_33","doi-asserted-by":"crossref","unstructured":"Duki\u0107, J., Re\u017eek Jambrak, A., Jurec, J., Merunka, D., Vali\u0107, S., Radi\u010di\u0107, R., Krstulovi\u0107, N., Nutrizio, M., and Dubrovi\u0107, I. (2025). High-power ultrasound and high-voltage electrical discharge-assisted extractions of bioactive compounds from sugar beet (Beta vulgaris L.) waste: Electron spin resonance and optical emission spectroscopy analysis. Molecules, 30.","DOI":"10.3390\/molecules30040796"},{"key":"ref_34","doi-asserted-by":"crossref","first-page":"110497","DOI":"10.1016\/j.microc.2024.110497","article-title":"Optimization of extraction condition to improve blackthorn (Prunus spinosa L.) polyphenols, anthocyanins and antioxidant activity by natural deep eutectic solvent (NADES) using the simplex lattice mixture design method","volume":"200","author":"Koraqi","year":"2024","journal-title":"Microchem. J."},{"key":"ref_35","doi-asserted-by":"crossref","unstructured":"Vega, E.N., Gonz\u00e1lez-Zamorano, L., Cebadera, E., Barros, L., Pires, T.C.S.P., Molina, A.K., da Silveira, T.F.F., Vidal-Diez de Ulzurrun, G., Tard\u00edo, J., and C\u00e1mara, M. (2025). Natural food colorant obtained from wild Berberis vulgaris L. by ultrasound-assisted extraction: Optimization and characterization. Foods, 14.","DOI":"10.3390\/foods14020183"},{"key":"ref_36","doi-asserted-by":"crossref","first-page":"106940","DOI":"10.1016\/j.ultsonch.2024.106940","article-title":"A simple new approach for mapping an ultrasonic tank for sonochemistry","volume":"107","author":"Mason","year":"2024","journal-title":"Ultrason. Sonochem."},{"key":"ref_37","doi-asserted-by":"crossref","unstructured":"Zaky, A.A., Witrowa-Rajchert, D., and Nowacka, M. (Food Saf. Health, 2025). Revolution of bioactive compound extraction: Impacts on food safety, health, and sustainability, Food Saf. Health, early view.","DOI":"10.1002\/fsh3.70012"},{"key":"ref_38","first-page":"2844","article-title":"Combined experimental design based-PROMETHEE approach to evaluate antimicrobial activity and optimization of polyphenol content of Prunus spinosa L","volume":"19","year":"2025","journal-title":"fruit. J. Food Meas. Charact."},{"key":"ref_39","doi-asserted-by":"crossref","unstructured":"Dr\u0103ghici-Popa, A.M., Boscornea, A.C., Brezoiu, A.M., Tomas, \u0218.T., P\u00e2rvulescu, O.C., and Stan, R. (2023). Effects of extraction process factors on the composition and antioxidant activity of blackthorn (Prunus spinosa L.) fruit extracts. Antioxidants, 12.","DOI":"10.3390\/antiox12101897"},{"key":"ref_40","doi-asserted-by":"crossref","unstructured":"Du, Y., Huang, P., Jin, W., Li, C., Yang, J., Wan, H., and He, Y. (2021). Optimization of extraction or purification process of multiple components from natural products: Entropy weight method combined with Plackett\u2013Burman design and central composite design. Molecules, 26.","DOI":"10.3390\/molecules26185572"},{"key":"ref_41","first-page":"123","article-title":"Preparation and characterization of compost tea derived from rockweed residues","volume":"86","author":"Egri","year":"2024","journal-title":"UPB Sci. Bull. Series B"},{"key":"ref_42","doi-asserted-by":"crossref","first-page":"834","DOI":"10.1016\/j.indcrop.2016.09.063","article-title":"An efficient homogenate-microwave-assisted extraction of flavonols and anthocyanins from blackcurrant marc: Optimization using combination of Plackett-Burman design and Box-Behnken design","volume":"94","author":"Li","year":"2016","journal-title":"Ind. Crops Prod."},{"key":"ref_43","doi-asserted-by":"crossref","unstructured":"Mo\u021b, A., P\u00e2rvulescu, O.C., Ion, V.A., Molo\u0219ag, A., Dobrin, A., B\u0103dulescu, L., Orbeci, C., Egri, D., Dobre, T., and L\u00f8es, A.-K. (2024). Preparation, characterization, and testing of compost tea derived from seaweed and fish residues. Agronomy, 14.","DOI":"10.3390\/agronomy14091919"},{"key":"ref_44","doi-asserted-by":"crossref","first-page":"3124","DOI":"10.1080\/10942912.2016.1274906","article-title":"Phenolic acids and flavonoids profiles of extracts from edible wild fruits and their antioxidant properties","volume":"20","author":"Cosmulescu","year":"2017","journal-title":"Int. J. Food Prop."},{"key":"ref_45","first-page":"279","article-title":"Total phenolics and antioxidant capacity assays of selected fruits","volume":"72","author":"Levaj","year":"2007","journal-title":"Agric. Conspec. Sci."},{"key":"ref_46","first-page":"89","article-title":"Physico-chemical characteristics of wild plum fruits (Prunus spinosa L.)","volume":"3","author":"Erturk","year":"2009","journal-title":"Int. J. Plant Prod."},{"key":"ref_47","doi-asserted-by":"crossref","first-page":"3721","DOI":"10.1016\/j.foodchem.2013.06.071","article-title":"Characterisation of phenolic compounds in wild fruits from Northeastern Portugal","volume":"141","author":"Barros","year":"2013","journal-title":"Food Chem."}],"container-title":["Antioxidants"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/www.mdpi.com\/2076-3921\/14\/6\/680\/pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2025,10,9]],"date-time":"2025-10-09T17:46:30Z","timestamp":1760031990000},"score":1,"resource":{"primary":{"URL":"https:\/\/www.mdpi.com\/2076-3921\/14\/6\/680"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2025,6,3]]},"references-count":47,"journal-issue":{"issue":"6","published-online":{"date-parts":[[2025,6]]}},"alternative-id":["antiox14060680"],"URL":"https:\/\/doi.org\/10.3390\/antiox14060680","relation":{},"ISSN":["2076-3921"],"issn-type":[{"value":"2076-3921","type":"electronic"}],"subject":[],"published":{"date-parts":[[2025,6,3]]}}}