{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,10,14]],"date-time":"2026-10-14T19:01:46Z","timestamp":1792004506372,"version":"4.4.0"},"reference-count":55,"publisher":"MDPI AG","issue":"11","license":[{"start":{"date-parts":[[2021,10,27]],"date-time":"2021-10-27T00:00:00Z","timestamp":1635292800000},"content-version":"vor","delay-in-days":0,"URL":"https:\/\/creativecommons.org\/licenses\/by\/4.0\/"}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Plants"],"abstract":"<jats:p>Rosemary (Rosmarinus officinalis L.) is known to be an effective potential source of natural antioxidants which confer benefits to human health. Their bioactive properties are mainly due to phenolic compounds but these molecules are highly vulnerable to oxidants, light, heat, pH, water and enzymatic activities. Therefore, the stability and shelf life of phenolic compounds should be increased by being protected from chemical and physical damage by means of encapsulation prior to application. Encapsulation is becoming increasingly important in the pharmaceutical, food, cosmetics, textile, personal care, chemical, biotechnology, and medicinal industries due to its potential for stabilization and delivery of delicate and precious bioactive compounds. The aim of the present work was to describe the polyphenolic profile of Tunisian Rosemary, collected from two different bioclimatic areas, and further loading in silk fibroin nanoparticles. The loaded nanoparticles were characterized in terms of morphology, size, polydispersity, Z-potential, secondary structure of the protein, encapsulation efficiency, loading content, and antioxidant activity. On one hand, HPLC analysis revealed the presence of 18 polyphenolic compounds of whichcarnosic acid and carnosol were found to be the most abundant compounds (46.3 to 76.4 and 22.4 to 43.5 mg of compound per gram of dry plant weight (mg\/g DPW) respectively), Total phenolic content (TPC) ranged from 85.8 to 137.3 mg of gallic acid equivalent (GAE)\/g DPW in post-distilled rosemary extracts andantioxidant activity reached the values of 5.9 to 8.3 \u00b5mol of ascorbic acid equivalent (AAE)\/g DPW). On the other hand loaded nanoparticles were almost spherical and presented nanometric size and negative Z-potential. Although the encapsulation efficiency in silk fibroin nanoparticles and the drug loading content were low in the conditions of the assay, the encapsulated polyphenols retained near 85% of the radical scavenging activity against DPPH\u00b7 after 24 h. of incubation at 37 \u00b0C. The results showed that post-distilled rosemary residues had an effective potential as natural antioxidants due to their significant antioxidant activity and seemed to be useful in both pharmaceutical and food industries with beneficial properties that might confer benefits to human health and these silk fibroin nanoparticles loaded with rosemary extracts are thus a promising combination for several applications in food technology or nanomedicine.<\/jats:p>","DOI":"10.3390\/plants10112312","type":"journal-article","created":{"date-parts":[[2021,10,27]],"date-time":"2021-10-27T23:24:42Z","timestamp":1635377082000},"page":"2312","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":56,"title":["Extraction and Encapsulation of Phenolic Compounds of Tunisian Rosemary (Rosmarinus officinalis L.) Extracts in Silk Fibroin Nanoparticles"],"prefix":"10.3390","volume":"10","author":[{"given":"Kheiria","family":"Hcini","sequence":"first","affiliation":[{"name":"Biodiversity, Biotechnology and Climate Change Laboratory (LR11ES09), Department of Life Sciences, Faculty of Science of Tunis, University of Tunis El Manar, Tunis 2092, Tunisia"},{"name":"Department of Life Sciences, Faculty of Sciences of Gafsa, University Campus Sidi Ahmed Zarroug, University of Gafsa, Gafsa 2112, Tunisia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-5749-3737","authenticated-orcid":false,"given":"Antonio A.","family":"Lozano-P\u00e9rez","sequence":"additional","affiliation":[{"name":"Departamento de Biotecnolog\u00eda, Gen\u00f3mica y Mejora Vegetal, Instituto Murciano de Investigaci\u00f3n y Desarrollo Agrario y Medioambiental (IMIDA), La Alberca, 30150 Murcia, Spain"},{"name":"Instituto Murciano de Investigaci\u00f3n Biosanitaria (IMIB)-Arrixaca, El Palmar, 30120 Murcia, Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jos\u00e9","family":"Luis Cenis","sequence":"additional","affiliation":[{"name":"Departamento de Biotecnolog\u00eda, Gen\u00f3mica y Mejora Vegetal, Instituto Murciano de Investigaci\u00f3n y Desarrollo Agrario y Medioambiental (IMIDA), La Alberca, 30150 Murcia, Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Mar\u00eda","family":"Qu\u00edlez","sequence":"additional","affiliation":[{"name":"Departamento de Desarrollo Rural, Enolog\u00eda y Agricultura Sostenible, Instituto Murciano de Investigaci\u00f3n y Desarrollo Agrario y Medioambiental (IMIDA), La Alberca, 30150 Murcia, Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-3523-4670","authenticated-orcid":false,"given":"Maria","family":"Jos\u00e9 Jord\u00e1n","sequence":"additional","affiliation":[{"name":"Departamento de Desarrollo Rural, Enolog\u00eda y Agricultura Sostenible, Instituto Murciano de Investigaci\u00f3n y Desarrollo Agrario y Medioambiental (IMIDA), La Alberca, 30150 Murcia, Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"1968","published-online":{"date-parts":[[2021,10,27]]},"reference":[{"key":"ref_1","unstructured":"Preedy, V.R. (2016). Rosemary (Rosmarinus officinalis L.) oils. Essential Oils in Food Preservation, Flavor and Safety, Elsevier. Chapter 77."},{"key":"ref_2","unstructured":"Institut National de Recherches en G\u00e9nie Rural, Eaux et For\u00eats, and Agence de Promotion des Investissements Agricoles (2006). Guide des Plantes M\u00e9dicinales et Aromatiques, INRGREF. APIA CN-CDI 2806."},{"key":"ref_3","doi-asserted-by":"crossref","unstructured":"Alu\u2019datt, M.H., Rababah, T., Alhamad, M.N., Gammoh, S., Al-Mahasneh, M.A., Tranchant, C.C., and Rawshdeh, M. (2018). Pharmaceutical, Nutraceutical and Therapeutic Properties of Selected Wild Medicinal Plants: Thyme, Spearmint, and Rosemary. Therapeutic, Probiotic, and Unconventional Foods, Academic Press. Chapter 15.","DOI":"10.1016\/B978-0-12-814625-5.00014-5"},{"key":"ref_4","doi-asserted-by":"crossref","first-page":"1491","DOI":"10.1016\/j.psj.2019.11.008","article-title":"Effect of natural extracts obtained from food industry by-products on nutritional quality and shelf life of chicken nuggets enriched with organic Zn and Se provided in broiler diet","volume":"99","author":"Ros","year":"2020","journal-title":"Poult. Sci."},{"key":"ref_5","doi-asserted-by":"crossref","first-page":"9603","DOI":"10.1021\/jf302881t","article-title":"Relevance of carnosic acid, carnosol, and rosmarinic acid concentrations in the in vitro antioxidant and antimicrobial activities of Rosmarinus officinalis (L.) methanolic extracts","volume":"60","author":"Lax","year":"2012","journal-title":"J. Agric. Food Chem."},{"key":"ref_6","doi-asserted-by":"crossref","first-page":"125688","DOI":"10.1016\/j.foodchem.2019.125688","article-title":"Comparative study of rosemary extracts and several synthetic and natural food antioxidants. Relevance of carnosic acid\/carnosol ratio","volume":"309","year":"2020","journal-title":"Food Chem."},{"key":"ref_7","doi-asserted-by":"crossref","first-page":"5165","DOI":"10.1021\/jf010697n","article-title":"Antioxidant activity and phenolic compounds in selected herbs","volume":"49","author":"Zheng","year":"2001","journal-title":"J. Agric. Food Chem."},{"key":"ref_8","doi-asserted-by":"crossref","first-page":"87","DOI":"10.1002\/pca.2717","article-title":"A Comprehensive Characterisation of Rosemary tea Obtained from Rosmarinus officinalis L. Collected in a sub-Humid Area of Tunisia","volume":"29","author":"Achour","year":"2018","journal-title":"Phytochem. Anal."},{"key":"ref_9","doi-asserted-by":"crossref","first-page":"112049","DOI":"10.1016\/j.indcrop.2019.112049","article-title":"Deep eutectic solvents applied in the extraction and stabilization of rosemary (Rosmarinus officinalis L.) phenolic compounds","volume":"144","author":"Barbieri","year":"2020","journal-title":"Ind. Crops Prod."},{"key":"ref_10","doi-asserted-by":"crossref","first-page":"5363","DOI":"10.1021\/jf100332w","article-title":"Flavonoids and phenolic compounds from rosmarinus officinalis","volume":"58","author":"Bai","year":"2010","journal-title":"J. Agric. Food Chem."},{"key":"ref_11","doi-asserted-by":"crossref","first-page":"616","DOI":"10.1016\/j.foodchem.2008.09.095","article-title":"Microencapsulation by spray drying of bioactive compounds from cactus pear (Opuntia ficusindica)","volume":"114","author":"Tapia","year":"2009","journal-title":"Food Chem."},{"key":"ref_12","first-page":"474","article-title":"Microencapsulation: Process, Techniques and Applications","volume":"2","author":"Umer","year":"2011","journal-title":"Int. J. Res. Pharm. Biomed. Sci."},{"key":"ref_13","doi-asserted-by":"crossref","first-page":"1361","DOI":"10.1081\/DRT-200063478","article-title":"Recent developments in microencapsulation of food ingredients","volume":"23","author":"Desai","year":"2005","journal-title":"Dry. Technol."},{"key":"ref_14","doi-asserted-by":"crossref","first-page":"1301","DOI":"10.1016\/j.indcrop.2010.10.002","article-title":"Black currant polyphenols: Their storage stability and microencapsulation","volume":"34","author":"Kolodziejczyk","year":"2011","journal-title":"Ind. Crops Prod."},{"key":"ref_15","first-page":"713","article-title":"Encapsulation of antioxidants by spray-drying","volume":"11","author":"Ferreira","year":"2007","journal-title":"Chem. Eng. Trans."},{"key":"ref_16","doi-asserted-by":"crossref","first-page":"11251","DOI":"10.1021\/jf801868h","article-title":"Storage stability of microencapsulated cloudberry (Rubus chamaemorus) phenolics","volume":"56","author":"Laine","year":"2008","journal-title":"J. Agric. Food Chem."},{"key":"ref_17","doi-asserted-by":"crossref","first-page":"528","DOI":"10.1126\/science.1188936","article-title":"New opportunities for an ancient material","volume":"309","author":"Omenetto","year":"2010","journal-title":"Science"},{"key":"ref_18","doi-asserted-by":"crossref","first-page":"381","DOI":"10.1016\/j.jconrel.2014.05.059","article-title":"Silk-based biomaterials for sustained drug delivery","volume":"190","author":"Yucel","year":"2014","journal-title":"J. Control. Release"},{"key":"ref_19","doi-asserted-by":"crossref","first-page":"401","DOI":"10.1016\/S0142-9612(02)00353-8","article-title":"Silk-based biomaterials","volume":"24","author":"Altman","year":"2003","journal-title":"Biomaterials"},{"key":"ref_20","doi-asserted-by":"crossref","first-page":"219","DOI":"10.1016\/j.jconrel.2005.12.009","article-title":"Silk fibroin as an organic polymer for controlled drug delivery","volume":"11","author":"Hofmann","year":"2006","journal-title":"J. Control. Release"},{"key":"ref_21","doi-asserted-by":"crossref","first-page":"312","DOI":"10.1002\/jemt.22606","article-title":"Preparation of silk fibroin carriers for controlled release","volume":"80","author":"Liu","year":"2015","journal-title":"Microsc. Res. Tech."},{"key":"ref_22","doi-asserted-by":"crossref","first-page":"161","DOI":"10.1016\/j.jconrel.2015.03.020","article-title":"Silk fibroin nanoparticle as a novel drug delivery system","volume":"206","author":"Mottaghitalab","year":"2015","journal-title":"J. Control. Release"},{"key":"ref_23","first-page":"4507","article-title":"Silk fibroin nanoparticles constitute a vector for controlled release of resveratrol in an experimental model of inflammatory bowel disease in rats","volume":"9","author":"Algieri","year":"2014","journal-title":"Int. J. Nanomed."},{"key":"ref_24","doi-asserted-by":"crossref","first-page":"11","DOI":"10.1016\/j.ijpharm.2016.12.046","article-title":"Silk fibroin nanoparticles: Efficient vehicles for the natural antioxidant quercetin","volume":"518","author":"Rivero","year":"2017","journal-title":"Int. J. Pharm."},{"key":"ref_25","doi-asserted-by":"crossref","unstructured":"Montalb\u00e1n, M., Coburn, J., Lozano-P\u00e9rez, A.A., Cenis, J.L., V\u00edllora, G., and Kaplan, D. (2018). Production of Curcumin-Loaded Silk Fibroin Nanoparticles for Cancer Therapy. Nanomaterials, 8.","DOI":"10.3390\/nano8020126"},{"key":"ref_26","doi-asserted-by":"crossref","first-page":"37","DOI":"10.1016\/j.ejpb.2019.02.008","article-title":"Silk fibroin nanoparticles for celecoxib and curcumin delivery: ROS-scavenging and anti-inflammatory activities in an in vitro model of osteoarthritis","volume":"137","author":"Crivelli","year":"2019","journal-title":"Eur. J. Pharm. Biopharm."},{"key":"ref_27","doi-asserted-by":"crossref","first-page":"793","DOI":"10.1007\/s11998-015-9668-1","article-title":"Encapsulation of volatile compounds in silk microparticles","volume":"12","author":"Elia","year":"2015","journal-title":"J. Coatings Technol. Res."},{"key":"ref_28","doi-asserted-by":"crossref","first-page":"1","DOI":"10.1002\/app.39990","article-title":"Encapsulation of oil in silk fibroin biomaterials","volume":"131","author":"Pritchard","year":"2014","journal-title":"J. Appl. Polym. Sci."},{"key":"ref_29","doi-asserted-by":"crossref","first-page":"1227","DOI":"10.1021\/jf062829o","article-title":"Adsorption of olive leaf (Olea europaea L.) antioxidants on silk fibroin","volume":"55","author":"Altiok","year":"2007","journal-title":"J. Agric. Food Chem."},{"key":"ref_30","doi-asserted-by":"crossref","first-page":"342","DOI":"10.1016\/j.seppur.2008.01.022","article-title":"Isolation of polyphenols from the extracts of olive leaves (Olea europaea L.) by adsorption on silk fibroin","volume":"62","author":"Altiok","year":"2008","journal-title":"Sep. Purif. Technol."},{"key":"ref_31","doi-asserted-by":"crossref","first-page":"9299","DOI":"10.14233\/ajchem.2013.15449","article-title":"Identification and Quantification of Phenolic Compounds of Tunisian Rosmarinus officinalis L.","volume":"25","author":"Hcini","year":"2013","journal-title":"Asian J. Chem."},{"key":"ref_32","doi-asserted-by":"crossref","first-page":"248","DOI":"10.1016\/j.tiv.2017.01.016","article-title":"Antioxidant activity of rosmarinic acid and its principal metabolites in chemical and cellular systems: Importance of physico-chemical characteristics","volume":"40","author":"Chan","year":"2017","journal-title":"Toxicol. Vitr."},{"key":"ref_33","doi-asserted-by":"crossref","first-page":"432","DOI":"10.1080\/10412905.2019.1577305","article-title":"Effect of bioclimatic area and season on phenolics and antioxidant activities of rosemary (Rosmarinus officinalis L.) leaves","volume":"31","author":"Yeddes","year":"2019","journal-title":"J. Essent. Oil Res."},{"key":"ref_34","doi-asserted-by":"crossref","first-page":"8062","DOI":"10.1021\/jf0712393","article-title":"Enhanced carnosic acid levels in two rosemary accessions exposed to cold stress conditions","volume":"55","author":"Luis","year":"2007","journal-title":"J. Agric. Food Chem."},{"key":"ref_35","first-page":"145","article-title":"Effect of the phenological stage on the chemical composition, and antimicrobial and antioxidant properties of Rosmarinus officinalis L. essential oil and its polyphenolic extract","volume":"29","author":"Lax","year":"2013","journal-title":"Ind. Crops Prod."},{"key":"ref_36","first-page":"12","article-title":"Exploitation of the biological potential of Satureja thymbra essential oil and distillation by-products","volume":"4","author":"Tsimogiannis","year":"2017","journal-title":"J. Appl. Res. Med. Aromat. Plants"},{"key":"ref_37","doi-asserted-by":"crossref","first-page":"1381","DOI":"10.1104\/pp.17.01183","article-title":"Carnosic acid and carnosol, two major antioxidants of rosemary, act through different mechanisms","volume":"175","author":"Loussouarn","year":"2017","journal-title":"Plant Physiol."},{"key":"ref_38","doi-asserted-by":"crossref","first-page":"37","DOI":"10.1186\/s13065-018-0387-4","article-title":"Comparison of the antioxidant effects of carnosic acid and synthetic antioxidants on tara seed oil","volume":"12","author":"Li","year":"2018","journal-title":"Chem. Cent. J."},{"key":"ref_39","doi-asserted-by":"crossref","first-page":"456253","DOI":"10.1155\/2013\/456253","article-title":"Rosmarinic acid-rich extracts of summer savory (Satureja hortensis L.) protect jurkat T cells against oxidative stress","volume":"2013","author":"Chkhikvishvili","year":"2013","journal-title":"Oxid. Med. Cell. Longev."},{"key":"ref_40","doi-asserted-by":"crossref","first-page":"FSO283","DOI":"10.4155\/fsoa-2017-0124","article-title":"Rosmarinus officinalis L.: An update review of its phytochemistry and biological activity","volume":"4","author":"Andrade","year":"2018","journal-title":"Futur. Sci. OA"},{"key":"ref_41","doi-asserted-by":"crossref","first-page":"808","DOI":"10.1038\/s41598-018-37173-7","article-title":"Rosemary (Rosmarinus officinalis) extract causes ROS-induced necrotic cell death and inhibits tumor growth in vivo","volume":"9","author":"Cifuentes","year":"2019","journal-title":"Sci. Rep."},{"key":"ref_42","first-page":"41702","article-title":"Production of silk fibroin nanoparticles using ionic liquids and high-power ultrasounds","volume":"132","author":"Cragnolini","year":"2014","journal-title":"J. Appl. Polym. Sci."},{"key":"ref_43","doi-asserted-by":"crossref","first-page":"13513","DOI":"10.1039\/C5DT00378D","article-title":"Antitumor properties of platinum (IV) prodrug-loaded silk fibroin nanoparticles","volume":"44","author":"Gil","year":"2015","journal-title":"Dalt. Trans."},{"key":"ref_44","doi-asserted-by":"crossref","first-page":"26","DOI":"10.1186\/1477-3155-11-26","article-title":"Interaction of nanoparticles with proteins: Relation to bio-reactivity of the nanoparticle","volume":"11","author":"Saptarshi","year":"2013","journal-title":"J. Nanobiotechnol."},{"key":"ref_45","doi-asserted-by":"crossref","first-page":"885","DOI":"10.1007\/s11051-006-9162-x","article-title":"Formation of silk fibroin nanoparticles in water-miscible organic solvent and their characterization","volume":"9","author":"Zhang","year":"2007","journal-title":"J. Nanoparticle Res."},{"key":"ref_46","doi-asserted-by":"crossref","first-page":"910","DOI":"10.1039\/b703139d","article-title":"The preparation of regenerated silk fibroin microspheres","volume":"3","author":"Cao","year":"2007","journal-title":"Soft Matter"},{"key":"ref_47","doi-asserted-by":"crossref","first-page":"6161","DOI":"10.1021\/ma0610109","article-title":"Determining beta-sheet crystallinity in fibrous proteins by thermal analysis and infrared spectroscopy","volume":"39","author":"Hu","year":"2006","journal-title":"Macromolecules"},{"key":"ref_48","doi-asserted-by":"crossref","first-page":"9305","DOI":"10.1021\/jf302179c","article-title":"Degradation study of carnosic acid, carnosol, rosmarinic acid, and rosemary extract (Rosmarinus officinalis L.) assessed using HPLC","volume":"60","author":"Zhang","year":"2012","journal-title":"J. Agric. Food Chem."},{"key":"ref_49","doi-asserted-by":"crossref","first-page":"6703","DOI":"10.1038\/s41598-019-43134-5","article-title":"Effect of different cocoon stifling methods on the properties of silk fibroin biomaterials","volume":"9","author":"Pagan","year":"2019","journal-title":"Sci. Rep."},{"key":"ref_50","doi-asserted-by":"crossref","first-page":"145","DOI":"10.1016\/j.indcrop.2008.04.021","article-title":"Polyphenolic extract and essential oil quality of Thymus zygis ssp. gracilis shrubs cultivated under different watering levels","volume":"29","author":"Sotomayor","year":"2009","journal-title":"Ind. Crops Prod."},{"key":"ref_51","doi-asserted-by":"crossref","first-page":"144","DOI":"10.5344\/ajev.1965.16.3.144","article-title":"Colorimetry to total phenolics with phosphomolybdic acid reagents","volume":"16","author":"Singleton","year":"1985","journal-title":"Am. J. Enol. Vinic."},{"key":"ref_52","doi-asserted-by":"crossref","first-page":"629","DOI":"10.1021\/jf00039a005","article-title":"Scavenging Effect of Methanolic Extracts of Peanut Hulls on Free-Radical and Active-Oxygen Species","volume":"42","author":"Yen","year":"1994","journal-title":"J. Agric. Food Chem."},{"key":"ref_53","doi-asserted-by":"crossref","unstructured":"Carissimi, G., Lozano-p\u00e9rez, A.A., Montalb\u00e1n, M.G., Aznar-Cervantes, S.D., Cenis, J.L., and Villora, G. (2019). Revealing the influence of the degumming process in the properties of silk fibroin nanoparticles. Polymers, 11.","DOI":"10.20944\/preprints201911.0049.v1"},{"key":"ref_54","first-page":"91","article-title":"Dissolution of silk fibroin with calcium chloride\/ethanol aqueous solution","volume":"67","author":"Ajisawa","year":"1998","journal-title":"J. Sericult. Sci. Japan."},{"key":"ref_55","doi-asserted-by":"crossref","first-page":"1","DOI":"10.1016\/j.colsurfb.2009.09.001","article-title":"Biodegradable polymeric nanoparticles based drug delivery systems","volume":"75","author":"Kumari","year":"2010","journal-title":"Colloids Surfaces B Biointerfaces"}],"container-title":["Plants"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/www.mdpi.com\/2223-7747\/10\/11\/2312\/pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2025,10,11]],"date-time":"2025-10-11T07:21:15Z","timestamp":1760167275000},"score":1,"resource":{"primary":{"URL":"https:\/\/www.mdpi.com\/2223-7747\/10\/11\/2312"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2021,10,27]]},"references-count":55,"journal-issue":{"issue":"11","published-online":{"date-parts":[[2021,11]]}},"alternative-id":["plants10112312"],"URL":"https:\/\/doi.org\/10.3390\/plants10112312","relation":{},"ISSN":["2223-7747"],"issn-type":[{"value":"2223-7747","type":"electronic"}],"subject":[],"published":{"date-parts":[[2021,10,27]]}}}