Green solvents and enzymes combined with advanced extraction techniques for the recovery of bioactive carotenoids and extractable/non-extractable polyphenols from grapefruit peels

The simultaneous extraction of extractable phenolic compounds (EPPs) and carotenoids from grapefruit peels using microwave-assisted extraction (MAE) with biobased solvents was optimized, followed by non-extractable polyphenols (NEPs) extraction. Ethyl acetate:γ-valerolactone (20:80 v/v) yielded the...

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Main Authors: Gloria Domínguez-Rodríguez, María Concepción García, María Luisa Marina
Format: Article
Language:English
Published: Elsevier 2025-08-01
Series:Advances in Sample Preparation
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Online Access:http://www.sciencedirect.com/science/article/pii/S2772582025000452
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author Gloria Domínguez-Rodríguez
María Concepción García
María Luisa Marina
author_facet Gloria Domínguez-Rodríguez
María Concepción García
María Luisa Marina
author_sort Gloria Domínguez-Rodríguez
collection DOAJ
description The simultaneous extraction of extractable phenolic compounds (EPPs) and carotenoids from grapefruit peels using microwave-assisted extraction (MAE) with biobased solvents was optimized, followed by non-extractable polyphenols (NEPs) extraction. Ethyl acetate:γ-valerolactone (20:80 v/v) yielded the highest antioxidant and anti-inflammatory EPPs at 50 °C in 6 min. From the residue, NEPs were obtained by comparing several methods: ultrasound-assisted extraction (UAE) combined with enzymatic-assisted extraction (EAE), and UAE and MAE with natural deep eutectic solvents (NaDES). UAE (15 min, 30 % amplitude) followed by EAE (70 °C, 40 min) and MAE-NaDES using choline chloride:lactic acid (1:2, 50 % water, 50 °C, 6 min) yielded the most bioactive NEPs. HPLC-DAD-QTOF-MS analysis allowed to identified 19 polyphenols in both extracts, highlighting naringin as the majority, particularly in UAE-EAE extract. Stability tests showed UAE-EAE extracts protect against oxidative damage, potentially extending the shelf life of food products. On the other hand, MAE-NaDES extracts prevent anti-inflammatory compound degradation, indicating their potential application in pharmaceutical formulations. Thus, depending on the purpose, either UAE-EAE or MAE-NaDES can be used.
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publishDate 2025-08-01
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spelling doaj-art-32f52a46c2bc4b7bb9beff3f046b6cf52025-08-20T03:10:51ZengElsevierAdvances in Sample Preparation2772-58202025-08-011510019210.1016/j.sampre.2025.100192Green solvents and enzymes combined with advanced extraction techniques for the recovery of bioactive carotenoids and extractable/non-extractable polyphenols from grapefruit peelsGloria Domínguez-Rodríguez0María Concepción García1María Luisa Marina2Universidad de Alcalá, Departamento de Química Analítica, Química Física e Ingeniería Química, Ctra. Madrid-Barcelona Km. 33.600, 28871 Alcalá de Henares, Madrid, SpainUniversidad de Alcalá, Departamento de Química Analítica, Química Física e Ingeniería Química, Ctra. Madrid-Barcelona Km. 33.600, 28871 Alcalá de Henares, Madrid, Spain; Universidad de Alcalá, Instituto de Investigación Química Andrés M. del Río, Ctra. Madrid-Barcelona Km. 33.600, 28871 Alcalá de Henares, Madrid, SpainUniversidad de Alcalá, Departamento de Química Analítica, Química Física e Ingeniería Química, Ctra. Madrid-Barcelona Km. 33.600, 28871 Alcalá de Henares, Madrid, Spain; Universidad de Alcalá, Instituto de Investigación Química Andrés M. del Río, Ctra. Madrid-Barcelona Km. 33.600, 28871 Alcalá de Henares, Madrid, Spain; Corresponding author.The simultaneous extraction of extractable phenolic compounds (EPPs) and carotenoids from grapefruit peels using microwave-assisted extraction (MAE) with biobased solvents was optimized, followed by non-extractable polyphenols (NEPs) extraction. Ethyl acetate:γ-valerolactone (20:80 v/v) yielded the highest antioxidant and anti-inflammatory EPPs at 50 °C in 6 min. From the residue, NEPs were obtained by comparing several methods: ultrasound-assisted extraction (UAE) combined with enzymatic-assisted extraction (EAE), and UAE and MAE with natural deep eutectic solvents (NaDES). UAE (15 min, 30 % amplitude) followed by EAE (70 °C, 40 min) and MAE-NaDES using choline chloride:lactic acid (1:2, 50 % water, 50 °C, 6 min) yielded the most bioactive NEPs. HPLC-DAD-QTOF-MS analysis allowed to identified 19 polyphenols in both extracts, highlighting naringin as the majority, particularly in UAE-EAE extract. Stability tests showed UAE-EAE extracts protect against oxidative damage, potentially extending the shelf life of food products. On the other hand, MAE-NaDES extracts prevent anti-inflammatory compound degradation, indicating their potential application in pharmaceutical formulations. Thus, depending on the purpose, either UAE-EAE or MAE-NaDES can be used.http://www.sciencedirect.com/science/article/pii/S2772582025000452Anti-inflammatoryAntioxidantBiobased solventsEnzymatic-assisted extractionMicrowave-assisted extractionUltrasonic-assisted extraction
spellingShingle Gloria Domínguez-Rodríguez
María Concepción García
María Luisa Marina
Green solvents and enzymes combined with advanced extraction techniques for the recovery of bioactive carotenoids and extractable/non-extractable polyphenols from grapefruit peels
Advances in Sample Preparation
Anti-inflammatory
Antioxidant
Biobased solvents
Enzymatic-assisted extraction
Microwave-assisted extraction
Ultrasonic-assisted extraction
title Green solvents and enzymes combined with advanced extraction techniques for the recovery of bioactive carotenoids and extractable/non-extractable polyphenols from grapefruit peels
title_full Green solvents and enzymes combined with advanced extraction techniques for the recovery of bioactive carotenoids and extractable/non-extractable polyphenols from grapefruit peels
title_fullStr Green solvents and enzymes combined with advanced extraction techniques for the recovery of bioactive carotenoids and extractable/non-extractable polyphenols from grapefruit peels
title_full_unstemmed Green solvents and enzymes combined with advanced extraction techniques for the recovery of bioactive carotenoids and extractable/non-extractable polyphenols from grapefruit peels
title_short Green solvents and enzymes combined with advanced extraction techniques for the recovery of bioactive carotenoids and extractable/non-extractable polyphenols from grapefruit peels
title_sort green solvents and enzymes combined with advanced extraction techniques for the recovery of bioactive carotenoids and extractable non extractable polyphenols from grapefruit peels
topic Anti-inflammatory
Antioxidant
Biobased solvents
Enzymatic-assisted extraction
Microwave-assisted extraction
Ultrasonic-assisted extraction
url http://www.sciencedirect.com/science/article/pii/S2772582025000452
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