An innovative approach for the recovery of nobiletin, hesperidin, and other phytochemicals from tangerine leaves (Citrus reticulata) by-products using a solvent mixture based on natural compounds

Citrus reticulata leaves, rich in phytochemicals, are underutilized by-products with sustainable valorization potential under Green Chemistry principles. This study developed an eco-friendly solvent combining thymol (Thy), oxalic acid (OA), and ethanol (EtOH) to extract nobiletin and hesperidin guid...

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Autores: Sorita, Guilherme Dallarmi, Rodríguez-García, Camilo, Strieder, Monique M., Domínguez-Rodríguez, Gloria, Montero, Lidia, Sanchez Bragagnolo, Felipe, Palomeque, Liliam, Parada-Alfonso, Fabián, Ibáñez, Elena
Formato: artículo
Estado:Versión aceptada para publicación
Fecha de publicación:2025
País:España
Recursos:Consejo Superior de Investigaciones Científicas (CSIC)
Repositorio:DIGITAL.CSIC. Repositorio Institucional del CSIC
OAI Identifier:oai:digital.csic.es:10261/391034
Acesso em linha:http://hdl.handle.net/10261/391034
Access Level:acceso embargado
Palavra-chave:Nobiletin
Hesperidin
Neuroprotective compounds
COSMO-RS
Thymol: Oxalic acid:Ethanol solvent
High-intensity ultrasound
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spelling An innovative approach for the recovery of nobiletin, hesperidin, and other phytochemicals from tangerine leaves (Citrus reticulata) by-products using a solvent mixture based on natural compoundsSorita, Guilherme DallarmiRodríguez-García, CamiloStrieder, Monique M.Domínguez-Rodríguez, GloriaMontero, LidiaSanchez Bragagnolo, FelipePalomeque, LiliamParada-Alfonso, FabiánIbáñez, ElenaNobiletinHesperidinNeuroprotective compoundsCOSMO-RSThymol: Oxalic acid:Ethanol solventHigh-intensity ultrasoundCitrus reticulata leaves, rich in phytochemicals, are underutilized by-products with sustainable valorization potential under Green Chemistry principles. This study developed an eco-friendly solvent combining thymol (Thy), oxalic acid (OA), and ethanol (EtOH) to extract nobiletin and hesperidin guided by COSMO-RS and high-intensity ultrasound (HIUS). The optimum solvent composition (0.9 % oxalic acid, 24.1 % thymol and 75 % EtOH) achieved higher yields of nobiletin (0.38 mg mL−1), hesperidin (0.74 mg mL−1) than pure EtOH (0.30 mg mL−1 of nobiletin and 0.64 mg mL−1 of hesperidin). HPLC-DAD-MS/MS and GC–MS analyses revealed that the optimized extract had a more complex phytochemical profile with a richer composition than the EtOH extract. Furthermore, optimized Thy-OA-EtOH extract exhibited superior bioactivity, with enhanced antioxidant capacity and neuroprotective effects (IC50: 334.40 mg mL−1) compared to HIUS-EtOH (IC50: 1482.20 mg mL−1). This study highlights the potential of natural compound mixtures with HIUS for extracting phytochemicals from citrus leaves for food and pharmaceutical applications.Authors acknowledge the funding from projects PID2020–113050RB-I00, and PDC2021–120814-I00 (MCIN/AEI/10.13039/501100011033 and The European Union Next GenerationEU/PRTR), and CSIC (INCGLO0019 - Bioprospection of local agricultural resources, a way to achieve the Objectives of Sustainable development). The authors are also thankfull for Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (88887.877048/2023-00, CAPES PRINT, Brazil), National Council for Scientific and Technological Development (CNPq, 150281/2024-2), and Fundação de Amparo à Pesquisa do Estado de São Paulo - FAPESP (grant number: 2023/05722-6, 2023/12621-1, 2022/10469-5). We are also thankful to the Universidad Nacional de Colombia (Hermes 57909).Peer reviewedElsevierAgencia Estatal de Investigación (España)Ministerio de Ciencia, Innovación y Universidades (España)European CommissionConsejo Superior de Investigaciones Científicas (España)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (Brasil)Fundação de Amparo à Pesquisa do Estado de São PauloConselho Nacional de Desenvolvimento Científico e Tecnológico (Brasil)Universidad Nacional de ColombiaConsejo Superior de Investigaciones Científicas [https://ror.org/02gfc7t72]202520252025info:eu-repo/semantics/articlehttp://purl.org/coar/resource_type/c_6501Postprintinfo:eu-repo/semantics/acceptedVersionapplication/pdfhttp://hdl.handle.net/10261/391034reponame:DIGITAL.CSIC. Repositorio Institucional del CSICinstname:Consejo Superior de Investigaciones Científicas (CSIC)Inglés#PLACEHOLDER_PARENT_METADATA_VALUE##PLACEHOLDER_PARENT_METADATA_VALUE#info:eu-repo/grantAgreement/AEI/Plan Estatal de Investigación Científica y Técnica y de Innovación 2017-2020/PID2020-113050RB-I00info:eu-repo/grantAgreement/AEI/Plan Estatal de Investigación Científica y Técnica y de Innovación 2017-2020/PDC2021-120814-I00The underlying dataset has been published as supplementary material of the article in the publisher platform at DOI 10.1016/j.foodchem.2025.144628https://doi.org/10.1016/j.foodchem.2025.144628Síinfo:eu-repo/semantics/embargoedAccessoai:digital.csic.es:10261/3910342026-05-22T06:33:51Z
dc.title.none.fl_str_mv An innovative approach for the recovery of nobiletin, hesperidin, and other phytochemicals from tangerine leaves (Citrus reticulata) by-products using a solvent mixture based on natural compounds
title An innovative approach for the recovery of nobiletin, hesperidin, and other phytochemicals from tangerine leaves (Citrus reticulata) by-products using a solvent mixture based on natural compounds
spellingShingle An innovative approach for the recovery of nobiletin, hesperidin, and other phytochemicals from tangerine leaves (Citrus reticulata) by-products using a solvent mixture based on natural compounds
Sorita, Guilherme Dallarmi
Nobiletin
Hesperidin
Neuroprotective compounds
COSMO-RS
Thymol: Oxalic acid:Ethanol solvent
High-intensity ultrasound
title_short An innovative approach for the recovery of nobiletin, hesperidin, and other phytochemicals from tangerine leaves (Citrus reticulata) by-products using a solvent mixture based on natural compounds
title_full An innovative approach for the recovery of nobiletin, hesperidin, and other phytochemicals from tangerine leaves (Citrus reticulata) by-products using a solvent mixture based on natural compounds
title_fullStr An innovative approach for the recovery of nobiletin, hesperidin, and other phytochemicals from tangerine leaves (Citrus reticulata) by-products using a solvent mixture based on natural compounds
title_full_unstemmed An innovative approach for the recovery of nobiletin, hesperidin, and other phytochemicals from tangerine leaves (Citrus reticulata) by-products using a solvent mixture based on natural compounds
title_sort An innovative approach for the recovery of nobiletin, hesperidin, and other phytochemicals from tangerine leaves (Citrus reticulata) by-products using a solvent mixture based on natural compounds
dc.creator.none.fl_str_mv Sorita, Guilherme Dallarmi
Rodríguez-García, Camilo
Strieder, Monique M.
Domínguez-Rodríguez, Gloria
Montero, Lidia
Sanchez Bragagnolo, Felipe
Palomeque, Liliam
Parada-Alfonso, Fabián
Ibáñez, Elena
author Sorita, Guilherme Dallarmi
author_facet Sorita, Guilherme Dallarmi
Rodríguez-García, Camilo
Strieder, Monique M.
Domínguez-Rodríguez, Gloria
Montero, Lidia
Sanchez Bragagnolo, Felipe
Palomeque, Liliam
Parada-Alfonso, Fabián
Ibáñez, Elena
author_role author
author2 Rodríguez-García, Camilo
Strieder, Monique M.
Domínguez-Rodríguez, Gloria
Montero, Lidia
Sanchez Bragagnolo, Felipe
Palomeque, Liliam
Parada-Alfonso, Fabián
Ibáñez, Elena
author2_role author
author
author
author
author
author
author
author
dc.contributor.none.fl_str_mv Agencia Estatal de Investigación (España)
Ministerio de Ciencia, Innovación y Universidades (España)
European Commission
Consejo Superior de Investigaciones Científicas (España)
Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (Brasil)
Fundação de Amparo à Pesquisa do Estado de São Paulo
Conselho Nacional de Desenvolvimento Científico e Tecnológico (Brasil)
Universidad Nacional de Colombia
Consejo Superior de Investigaciones Científicas [https://ror.org/02gfc7t72]
dc.subject.none.fl_str_mv Nobiletin
Hesperidin
Neuroprotective compounds
COSMO-RS
Thymol: Oxalic acid:Ethanol solvent
High-intensity ultrasound
topic Nobiletin
Hesperidin
Neuroprotective compounds
COSMO-RS
Thymol: Oxalic acid:Ethanol solvent
High-intensity ultrasound
description Citrus reticulata leaves, rich in phytochemicals, are underutilized by-products with sustainable valorization potential under Green Chemistry principles. This study developed an eco-friendly solvent combining thymol (Thy), oxalic acid (OA), and ethanol (EtOH) to extract nobiletin and hesperidin guided by COSMO-RS and high-intensity ultrasound (HIUS). The optimum solvent composition (0.9 % oxalic acid, 24.1 % thymol and 75 % EtOH) achieved higher yields of nobiletin (0.38 mg mL−1), hesperidin (0.74 mg mL−1) than pure EtOH (0.30 mg mL−1 of nobiletin and 0.64 mg mL−1 of hesperidin). HPLC-DAD-MS/MS and GC–MS analyses revealed that the optimized extract had a more complex phytochemical profile with a richer composition than the EtOH extract. Furthermore, optimized Thy-OA-EtOH extract exhibited superior bioactivity, with enhanced antioxidant capacity and neuroprotective effects (IC50: 334.40 mg mL−1) compared to HIUS-EtOH (IC50: 1482.20 mg mL−1). This study highlights the potential of natural compound mixtures with HIUS for extracting phytochemicals from citrus leaves for food and pharmaceutical applications.
publishDate 2025
dc.date.none.fl_str_mv 2025
2025
2025
dc.type.none.fl_str_mv info:eu-repo/semantics/article
http://purl.org/coar/resource_type/c_6501
Postprint
info:eu-repo/semantics/acceptedVersion
format article
status_str acceptedVersion
dc.identifier.none.fl_str_mv http://hdl.handle.net/10261/391034
url http://hdl.handle.net/10261/391034
dc.language.none.fl_str_mv Inglés
language_invalid_str_mv Inglés
dc.relation.none.fl_str_mv #PLACEHOLDER_PARENT_METADATA_VALUE#
#PLACEHOLDER_PARENT_METADATA_VALUE#
info:eu-repo/grantAgreement/AEI/Plan Estatal de Investigación Científica y Técnica y de Innovación 2017-2020/PID2020-113050RB-I00
info:eu-repo/grantAgreement/AEI/Plan Estatal de Investigación Científica y Técnica y de Innovación 2017-2020/PDC2021-120814-I00
The underlying dataset has been published as supplementary material of the article in the publisher platform at DOI 10.1016/j.foodchem.2025.144628
https://doi.org/10.1016/j.foodchem.2025.144628

dc.rights.none.fl_str_mv info:eu-repo/semantics/embargoedAccess
eu_rights_str_mv embargoedAccess
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dc.publisher.none.fl_str_mv Elsevier
publisher.none.fl_str_mv Elsevier
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instname:Consejo Superior de Investigaciones Científicas (CSIC)
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