Isolation of Polyphenols from Aqueous Extract of the Halophyte <i>Salicornia ramosissima</i>

Polyphenols from residual non-food grade <i>Salicornia ramosissima</i> have health-promoting effects in feed, food, or nutraceutical applications. Therefore, the isolation of polyphenols is of interest from a series of environmentally friendly isolation methods with recyclable solvents....

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Main Authors: Malthe Fredsgaard, Job Tchoumtchoua, Stephan Kohnen, Tanmay Chaturvedi, Mette Hedegaard Thomsen
Format: Article
Language:English
Published: MDPI AG 2023-12-01
Series:Molecules
Subjects:
Online Access:https://www.mdpi.com/1420-3049/29/1/220
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author Malthe Fredsgaard
Job Tchoumtchoua
Stephan Kohnen
Tanmay Chaturvedi
Mette Hedegaard Thomsen
author_facet Malthe Fredsgaard
Job Tchoumtchoua
Stephan Kohnen
Tanmay Chaturvedi
Mette Hedegaard Thomsen
author_sort Malthe Fredsgaard
collection DOAJ
description Polyphenols from residual non-food grade <i>Salicornia ramosissima</i> have health-promoting effects in feed, food, or nutraceutical applications. Therefore, the isolation of polyphenols is of interest from a series of environmentally friendly isolation methods with recyclable solvents. The isolation of polyphenols from non-food grade <i>S. ramosissima</i> was investigated using sequential membrane filtration with and without acid pretreatment, liquid–liquid extraction, resin adsorption, and centrifugal partition chromatography (CPC); analyzed by the Folin–Ciocalteu assay for total polyphenols; and finally analyzed using UPLC-TQMS in negative ion-spray mode for detection of 14 polyphenols. Sequential membrane filtration and acid hydrolysis indicated the polyphenols forming complexes with other compounds, retaining the polyphenols in the retentate fraction of large molecular weight cut-off membrane sizes. Conventional liquid–liquid extraction using sequential ethyl acetate and n-butanol showed most polyphenols were extracted, apart from chlorogenic acids, indicating a low isolation efficiency of higher polarity polyphenols. Analysis of the extract after resin adsorption by Amberlite XAD-4 resin showed high efficiency for separation, with 100% of polyphenols adsorbed to the resin after 13 bed volumes and 96.7% eluted from the resin using ethanol. CPC fractionations were performed to fractionate the concentrated extract after resin adsorption. CPC fractionations of the 14 polyphenols were performed using an organic or aqueous phase as a mobile phase. Depending on the mobile phase, different compounds were isolated in a high concentration. Using these easily scalable methods, it was possible to comprehensively study the polyphenols of interest from <i>S. ramosissima</i> and their isolation mechanics. This study will potentially lead the way for the large-scale isolation of polyphenols from <i>S. ramosissima</i> and other complex halophytes. The compounds of the highest concentration after CPC fractionation were isoquercitrin and hyperoside (155.27 mg/g), chlorogenic acid (85.54 mg/g), cryptochlorogenic acid (101.50 mg/g), and protocatechuic acid (398.67 mg/g), and further isolation using CPC could potentially yield novel polyphenol nutraceuticals.
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spelling doaj.art-1f8ecb444b2f46a98cf7f8332ba5b6342024-01-10T15:04:32ZengMDPI AGMolecules1420-30492023-12-0129122010.3390/molecules29010220Isolation of Polyphenols from Aqueous Extract of the Halophyte <i>Salicornia ramosissima</i>Malthe Fredsgaard0Job Tchoumtchoua1Stephan Kohnen2Tanmay Chaturvedi3Mette Hedegaard Thomsen4AAU Energy, Aalborg University, 6700 Esbjerg, DenmarkBiomass Valorisation Platform, CELABOR Scrl, 4650 Herve, BelgiumBiomass Valorisation Platform, CELABOR Scrl, 4650 Herve, BelgiumAAU Energy, Aalborg University, 6700 Esbjerg, DenmarkAAU Energy, Aalborg University, 6700 Esbjerg, DenmarkPolyphenols from residual non-food grade <i>Salicornia ramosissima</i> have health-promoting effects in feed, food, or nutraceutical applications. Therefore, the isolation of polyphenols is of interest from a series of environmentally friendly isolation methods with recyclable solvents. The isolation of polyphenols from non-food grade <i>S. ramosissima</i> was investigated using sequential membrane filtration with and without acid pretreatment, liquid–liquid extraction, resin adsorption, and centrifugal partition chromatography (CPC); analyzed by the Folin–Ciocalteu assay for total polyphenols; and finally analyzed using UPLC-TQMS in negative ion-spray mode for detection of 14 polyphenols. Sequential membrane filtration and acid hydrolysis indicated the polyphenols forming complexes with other compounds, retaining the polyphenols in the retentate fraction of large molecular weight cut-off membrane sizes. Conventional liquid–liquid extraction using sequential ethyl acetate and n-butanol showed most polyphenols were extracted, apart from chlorogenic acids, indicating a low isolation efficiency of higher polarity polyphenols. Analysis of the extract after resin adsorption by Amberlite XAD-4 resin showed high efficiency for separation, with 100% of polyphenols adsorbed to the resin after 13 bed volumes and 96.7% eluted from the resin using ethanol. CPC fractionations were performed to fractionate the concentrated extract after resin adsorption. CPC fractionations of the 14 polyphenols were performed using an organic or aqueous phase as a mobile phase. Depending on the mobile phase, different compounds were isolated in a high concentration. Using these easily scalable methods, it was possible to comprehensively study the polyphenols of interest from <i>S. ramosissima</i> and their isolation mechanics. This study will potentially lead the way for the large-scale isolation of polyphenols from <i>S. ramosissima</i> and other complex halophytes. The compounds of the highest concentration after CPC fractionation were isoquercitrin and hyperoside (155.27 mg/g), chlorogenic acid (85.54 mg/g), cryptochlorogenic acid (101.50 mg/g), and protocatechuic acid (398.67 mg/g), and further isolation using CPC could potentially yield novel polyphenol nutraceuticals.https://www.mdpi.com/1420-3049/29/1/220<i>Salicornia ramosissima</i>isolationpurificationpolyphenolsliquid–liquid extractionresin adsorption
spellingShingle Malthe Fredsgaard
Job Tchoumtchoua
Stephan Kohnen
Tanmay Chaturvedi
Mette Hedegaard Thomsen
Isolation of Polyphenols from Aqueous Extract of the Halophyte <i>Salicornia ramosissima</i>
Molecules
<i>Salicornia ramosissima</i>
isolation
purification
polyphenols
liquid–liquid extraction
resin adsorption
title Isolation of Polyphenols from Aqueous Extract of the Halophyte <i>Salicornia ramosissima</i>
title_full Isolation of Polyphenols from Aqueous Extract of the Halophyte <i>Salicornia ramosissima</i>
title_fullStr Isolation of Polyphenols from Aqueous Extract of the Halophyte <i>Salicornia ramosissima</i>
title_full_unstemmed Isolation of Polyphenols from Aqueous Extract of the Halophyte <i>Salicornia ramosissima</i>
title_short Isolation of Polyphenols from Aqueous Extract of the Halophyte <i>Salicornia ramosissima</i>
title_sort isolation of polyphenols from aqueous extract of the halophyte i salicornia ramosissima i
topic <i>Salicornia ramosissima</i>
isolation
purification
polyphenols
liquid–liquid extraction
resin adsorption
url https://www.mdpi.com/1420-3049/29/1/220
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