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Article

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

by
Branimir Pavlić
1,*,
Živan Mrkonjić
1,
Nemanja Teslić
2,
Aleksandra Cvetanović Kljakić
1,
Milica Pojić
2,
Anamarija Mandić
2,
Alena Stupar
2,
Filipa Santos
3,
Ana Rita C. Duarte
3 and
Aleksandra Mišan
2,*
1
Faculty of Technology, University of Novi Sad, Blvd. cara Lazara 1, 21000 Novi Sad, Serbia
2
Institute of Food Technology, University of Novi Sad, Blvd. cara Lazara 1, 21000 Novi Sad, Serbia
3
LAQV, REQUIMTE, Departamento de Química, Nova School of Science and Technology, 2829-516 Caparica, Portugal
*
Authors to whom correspondence should be addressed.
Molecules 2022, 27(5), 1508; https://doi.org/10.3390/molecules27051508
Submission received: 25 January 2022 / Revised: 11 February 2022 / Accepted: 15 February 2022 / Published: 23 February 2022
(This article belongs to the Special Issue Conventional and Emerging Extraction Techniques for Compounds from Natural Source and Food)
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Abstract

Wild thyme (Thymus serpyllum 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 l-proline (Pro)–glycerine (Gly) based solvents provided the best results. Preliminary experiments organized by 25−1 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–H2O; 1:2:1) were confirmed by the 1H-NMR.
Keywords: Thymus serpyllum L.; NADES; polyphenols; antioxidant activity; RSM optimization Thymus serpyllum L.; NADES; polyphenols; antioxidant activity; RSM optimization

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MDPI and ACS Style

Pavlić, B.; Mrkonjić, Ž.; Teslić, N.; Kljakić, A.C.; Pojić, M.; Mandić, A.; Stupar, A.; Santos, F.; Duarte, A.R.C.; Mišan, A. Natural Deep Eutectic Solvent (NADES) Extraction Improves Polyphenol Yield and Antioxidant Activity of Wild Thyme (Thymus serpyllum L.) Extracts. Molecules 2022, 27, 1508. https://doi.org/10.3390/molecules27051508

AMA Style

Pavlić B, Mrkonjić Ž, Teslić N, Kljakić AC, Pojić M, Mandić A, Stupar A, Santos F, Duarte ARC, Mišan A. Natural Deep Eutectic Solvent (NADES) Extraction Improves Polyphenol Yield and Antioxidant Activity of Wild Thyme (Thymus serpyllum L.) Extracts. Molecules. 2022; 27(5):1508. https://doi.org/10.3390/molecules27051508

Chicago/Turabian Style

Pavlić, Branimir, Živan Mrkonjić, Nemanja Teslić, Aleksandra Cvetanović Kljakić, Milica Pojić, Anamarija Mandić, Alena Stupar, Filipa Santos, Ana Rita C. Duarte, and Aleksandra Mišan. 2022. "Natural Deep Eutectic Solvent (NADES) Extraction Improves Polyphenol Yield and Antioxidant Activity of Wild Thyme (Thymus serpyllum L.) Extracts" Molecules 27, no. 5: 1508. https://doi.org/10.3390/molecules27051508

APA Style

Pavlić, B., Mrkonjić, Ž., Teslić, N., Kljakić, A. C., Pojić, M., Mandić, A., Stupar, A., Santos, F., Duarte, A. R. C., & Mišan, A. (2022). Natural Deep Eutectic Solvent (NADES) Extraction Improves Polyphenol Yield and Antioxidant Activity of Wild Thyme (Thymus serpyllum L.) Extracts. Molecules, 27(5), 1508. https://doi.org/10.3390/molecules27051508

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