Natural Deep Eutectic Solvent (NADES) Extraction Improves Polyphenol Yield and Antioxidant Activity of Wild Thyme (<i>Thymus serpyllum</i> L.) Extracts

Wild thyme (<i>Thymus serpyllum</i> L.) herbal dust has been recognized as a potential underutilized resource for the recovery of antioxidants. The aim of this paper was to optimize natural deep eutectic solvent (NADES) extraction of polyphenols to obtain improved antioxidant activity of...

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Main Authors: Branimir Pavlić, Živan Mrkonjić, Nemanja Teslić, Aleksandra Cvetanović Kljakić, Milica Pojić, Anamarija Mandić, Alena Stupar, Filipa Santos, Ana Rita C. Duarte, Aleksandra Mišan
Format: Article
Jezik:English
Izdano: MDPI AG 2022-02-01
Serija:Molecules
Teme:
Online dostop:https://www.mdpi.com/1420-3049/27/5/1508
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author Branimir Pavlić
Živan Mrkonjić
Nemanja Teslić
Aleksandra Cvetanović Kljakić
Milica Pojić
Anamarija Mandić
Alena Stupar
Filipa Santos
Ana Rita C. Duarte
Aleksandra Mišan
author_facet Branimir Pavlić
Živan Mrkonjić
Nemanja Teslić
Aleksandra Cvetanović Kljakić
Milica Pojić
Anamarija Mandić
Alena Stupar
Filipa Santos
Ana Rita C. Duarte
Aleksandra Mišan
author_sort Branimir Pavlić
collection DOAJ
description Wild thyme (<i>Thymus serpyllum</i> L.) herbal dust has been recognized as a potential underutilized resource for the recovery of antioxidants. The aim of this paper was to optimize natural deep eutectic solvent (NADES) extraction of polyphenols to obtain improved antioxidant activity of extracts determined by selected in vitro assays (DPPH, FRAP, and ABTS). Twenty different NADES systems were investigated in the first step of the screening of the extraction solvent and <span style="font-variant: small-caps;">l</span>-proline (Pro)–glycerine (Gly) based solvents provided the best results. Preliminary experiments organized by 2<sup>5−1</sup> fractional factorial design narrowed down the number of extraction factors from five (temperature, extraction time, NADES type, water content and L/S ratio) to three and determined their experimental domain for the final step. A face-centered central composite design with temperature (40–55–70 °C), extraction time (60–120–180 min) and L/S ratio (10–20–30 g NADES/g sample) was applied for influence analysis and process optimization. Multi-response optimization suggested a temperature of 65 °C, time of extraction of 180 min and L/S ratio of 28 g NADES/g DW as optimal extraction parameters. Experimental validation confirmed good agreement between experimental and predicted results in the extract obtained at optimal conditions and the interactions in the most suitable NADES (N16; Pro–Gly–H<sub>2</sub>O; 1:2:1) were confirmed by the <sup>1</sup>H-NMR.
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spelling doaj.art-14a5cac4f40b407b846e32c350edc7112023-11-23T23:25:23ZengMDPI AGMolecules1420-30492022-02-01275150810.3390/molecules27051508Natural Deep Eutectic Solvent (NADES) Extraction Improves Polyphenol Yield and Antioxidant Activity of Wild Thyme (<i>Thymus serpyllum</i> L.) ExtractsBranimir Pavlić0Živan Mrkonjić1Nemanja Teslić2Aleksandra Cvetanović Kljakić3Milica Pojić4Anamarija Mandić5Alena Stupar6Filipa Santos7Ana Rita C. Duarte8Aleksandra Mišan9Faculty of Technology, University of Novi Sad, Blvd. cara Lazara 1, 21000 Novi Sad, SerbiaFaculty of Technology, University of Novi Sad, Blvd. cara Lazara 1, 21000 Novi Sad, SerbiaInstitute of Food Technology, University of Novi Sad, Blvd. cara Lazara 1, 21000 Novi Sad, SerbiaFaculty of Technology, University of Novi Sad, Blvd. cara Lazara 1, 21000 Novi Sad, SerbiaInstitute of Food Technology, University of Novi Sad, Blvd. cara Lazara 1, 21000 Novi Sad, SerbiaInstitute of Food Technology, University of Novi Sad, Blvd. cara Lazara 1, 21000 Novi Sad, SerbiaInstitute of Food Technology, University of Novi Sad, Blvd. cara Lazara 1, 21000 Novi Sad, SerbiaLAQV, REQUIMTE, Departamento de Química, Nova School of Science and Technology, 2829-516 Caparica, PortugalLAQV, REQUIMTE, Departamento de Química, Nova School of Science and Technology, 2829-516 Caparica, PortugalInstitute of Food Technology, University of Novi Sad, Blvd. cara Lazara 1, 21000 Novi Sad, SerbiaWild thyme (<i>Thymus serpyllum</i> L.) herbal dust has been recognized as a potential underutilized resource for the recovery of antioxidants. The aim of this paper was to optimize natural deep eutectic solvent (NADES) extraction of polyphenols to obtain improved antioxidant activity of extracts determined by selected in vitro assays (DPPH, FRAP, and ABTS). Twenty different NADES systems were investigated in the first step of the screening of the extraction solvent and <span style="font-variant: small-caps;">l</span>-proline (Pro)–glycerine (Gly) based solvents provided the best results. Preliminary experiments organized by 2<sup>5−1</sup> fractional factorial design narrowed down the number of extraction factors from five (temperature, extraction time, NADES type, water content and L/S ratio) to three and determined their experimental domain for the final step. A face-centered central composite design with temperature (40–55–70 °C), extraction time (60–120–180 min) and L/S ratio (10–20–30 g NADES/g sample) was applied for influence analysis and process optimization. Multi-response optimization suggested a temperature of 65 °C, time of extraction of 180 min and L/S ratio of 28 g NADES/g DW as optimal extraction parameters. Experimental validation confirmed good agreement between experimental and predicted results in the extract obtained at optimal conditions and the interactions in the most suitable NADES (N16; Pro–Gly–H<sub>2</sub>O; 1:2:1) were confirmed by the <sup>1</sup>H-NMR.https://www.mdpi.com/1420-3049/27/5/1508<i>Thymus serpyllum</i> L.NADESpolyphenolsantioxidant activityRSM optimization
spellingShingle Branimir Pavlić
Živan Mrkonjić
Nemanja Teslić
Aleksandra Cvetanović Kljakić
Milica Pojić
Anamarija Mandić
Alena Stupar
Filipa Santos
Ana Rita C. Duarte
Aleksandra Mišan
Natural Deep Eutectic Solvent (NADES) Extraction Improves Polyphenol Yield and Antioxidant Activity of Wild Thyme (<i>Thymus serpyllum</i> L.) Extracts
Molecules
<i>Thymus serpyllum</i> L.
NADES
polyphenols
antioxidant activity
RSM optimization
title Natural Deep Eutectic Solvent (NADES) Extraction Improves Polyphenol Yield and Antioxidant Activity of Wild Thyme (<i>Thymus serpyllum</i> L.) Extracts
title_full Natural Deep Eutectic Solvent (NADES) Extraction Improves Polyphenol Yield and Antioxidant Activity of Wild Thyme (<i>Thymus serpyllum</i> L.) Extracts
title_fullStr Natural Deep Eutectic Solvent (NADES) Extraction Improves Polyphenol Yield and Antioxidant Activity of Wild Thyme (<i>Thymus serpyllum</i> L.) Extracts
title_full_unstemmed Natural Deep Eutectic Solvent (NADES) Extraction Improves Polyphenol Yield and Antioxidant Activity of Wild Thyme (<i>Thymus serpyllum</i> L.) Extracts
title_short Natural Deep Eutectic Solvent (NADES) Extraction Improves Polyphenol Yield and Antioxidant Activity of Wild Thyme (<i>Thymus serpyllum</i> L.) Extracts
title_sort natural deep eutectic solvent nades extraction improves polyphenol yield and antioxidant activity of wild thyme i thymus serpyllum i l extracts
topic <i>Thymus serpyllum</i> L.
NADES
polyphenols
antioxidant activity
RSM optimization
url https://www.mdpi.com/1420-3049/27/5/1508
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