Fractionation of a Procyanidin-Rich Grape Seed Extract by a Preparative Integrated Ultrafiltration/Reverse Osmosis/Solid-Phase Extraction Procedure

The consumption of grape seed extracts is known for its contribution to animal and human health and is associated with its relevant procyanidin content. However, there is a little scientific unanimity whether these properties are due to the procyanidin content or to the length of their polymers. The...

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Main Authors: Esperanza Guerrero-Hurtado, Alba Gutiérrez-Docio, Rebeca Fiedorowicz, Marin Prodanov
Format: Article
Language:English
Published: MDPI AG 2025-03-01
Series:Membranes
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Online Access:https://www.mdpi.com/2077-0375/15/3/92
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author Esperanza Guerrero-Hurtado
Alba Gutiérrez-Docio
Rebeca Fiedorowicz
Marin Prodanov
author_facet Esperanza Guerrero-Hurtado
Alba Gutiérrez-Docio
Rebeca Fiedorowicz
Marin Prodanov
author_sort Esperanza Guerrero-Hurtado
collection DOAJ
description The consumption of grape seed extracts is known for its contribution to animal and human health and is associated with its relevant procyanidin content. However, there is a little scientific unanimity whether these properties are due to the procyanidin content or to the length of their polymers. The main reason for this doubt is the technical difficulties related to their separation. Therefore, a preparative separation of grape seed extract was carried out using an integrated ultra/diafiltration procedure with membranes of 300, 30, 5, and 1 kDa molecular mass cut-offs, reverse osmosis and solid-phase extraction to obtain fractions of very high (>300 kDa), high (300–30 kDa), intermediate (30–5 kDa), low molecular mass (5–1 kDa), very-low-mass polar molecules and ions (<1 kDa), and very-low-mass dipole molecules (<1 kDa). Process parameters, mass transfer across the membranes and the quality of separation of each fraction are described and discussed in depth. A high degree of purification was achieved for the higher-molecular-mass fractions (>300, 300–30, and 30–5 kDa), as well as the big majority of procyanidin polymers and oligomers from very-low-molecular-mass species. All fractions were characterized for their procyanidin content by normal phase high-performance liquid chromatography coupled to a photodiode array detector (NP-HPLC-PAD). This analytical technique has shown for the first time that not only do oligomeric procyanidins elute at an increasing order of elution, but polymeric ones also do the same.
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spelling doaj-art-668c29b6e72f4df59924fd038feb9d502025-08-20T02:42:22ZengMDPI AGMembranes2077-03752025-03-011539210.3390/membranes15030092Fractionation of a Procyanidin-Rich Grape Seed Extract by a Preparative Integrated Ultrafiltration/Reverse Osmosis/Solid-Phase Extraction ProcedureEsperanza Guerrero-Hurtado0Alba Gutiérrez-Docio1Rebeca Fiedorowicz2Marin Prodanov3Departamento de Producción y Caracterización de Nuevos Alimentos, Instituto de Investigación en Ciencias de la Alimentación (CIAL) (CSIC-UAM), Calle Nicolás Cabrera, 9, Campus de Cantoblanco, Universidad Autónoma de Madrid, 28049 Madrid, SpainDepartamento de Producción y Caracterización de Nuevos Alimentos, Instituto de Investigación en Ciencias de la Alimentación (CIAL) (CSIC-UAM), Calle Nicolás Cabrera, 9, Campus de Cantoblanco, Universidad Autónoma de Madrid, 28049 Madrid, SpainDepartamento de Producción y Caracterización de Nuevos Alimentos, Instituto de Investigación en Ciencias de la Alimentación (CIAL) (CSIC-UAM), Calle Nicolás Cabrera, 9, Campus de Cantoblanco, Universidad Autónoma de Madrid, 28049 Madrid, SpainDepartamento de Producción y Caracterización de Nuevos Alimentos, Instituto de Investigación en Ciencias de la Alimentación (CIAL) (CSIC-UAM), Calle Nicolás Cabrera, 9, Campus de Cantoblanco, Universidad Autónoma de Madrid, 28049 Madrid, SpainThe consumption of grape seed extracts is known for its contribution to animal and human health and is associated with its relevant procyanidin content. However, there is a little scientific unanimity whether these properties are due to the procyanidin content or to the length of their polymers. The main reason for this doubt is the technical difficulties related to their separation. Therefore, a preparative separation of grape seed extract was carried out using an integrated ultra/diafiltration procedure with membranes of 300, 30, 5, and 1 kDa molecular mass cut-offs, reverse osmosis and solid-phase extraction to obtain fractions of very high (>300 kDa), high (300–30 kDa), intermediate (30–5 kDa), low molecular mass (5–1 kDa), very-low-mass polar molecules and ions (<1 kDa), and very-low-mass dipole molecules (<1 kDa). Process parameters, mass transfer across the membranes and the quality of separation of each fraction are described and discussed in depth. A high degree of purification was achieved for the higher-molecular-mass fractions (>300, 300–30, and 30–5 kDa), as well as the big majority of procyanidin polymers and oligomers from very-low-molecular-mass species. All fractions were characterized for their procyanidin content by normal phase high-performance liquid chromatography coupled to a photodiode array detector (NP-HPLC-PAD). This analytical technique has shown for the first time that not only do oligomeric procyanidins elute at an increasing order of elution, but polymeric ones also do the same.https://www.mdpi.com/2077-0375/15/3/92grape seed extractprocyanidin fractionationpreparative ultrafiltrationreverse osmosispreparative solid-phase extraction
spellingShingle Esperanza Guerrero-Hurtado
Alba Gutiérrez-Docio
Rebeca Fiedorowicz
Marin Prodanov
Fractionation of a Procyanidin-Rich Grape Seed Extract by a Preparative Integrated Ultrafiltration/Reverse Osmosis/Solid-Phase Extraction Procedure
Membranes
grape seed extract
procyanidin fractionation
preparative ultrafiltration
reverse osmosis
preparative solid-phase extraction
title Fractionation of a Procyanidin-Rich Grape Seed Extract by a Preparative Integrated Ultrafiltration/Reverse Osmosis/Solid-Phase Extraction Procedure
title_full Fractionation of a Procyanidin-Rich Grape Seed Extract by a Preparative Integrated Ultrafiltration/Reverse Osmosis/Solid-Phase Extraction Procedure
title_fullStr Fractionation of a Procyanidin-Rich Grape Seed Extract by a Preparative Integrated Ultrafiltration/Reverse Osmosis/Solid-Phase Extraction Procedure
title_full_unstemmed Fractionation of a Procyanidin-Rich Grape Seed Extract by a Preparative Integrated Ultrafiltration/Reverse Osmosis/Solid-Phase Extraction Procedure
title_short Fractionation of a Procyanidin-Rich Grape Seed Extract by a Preparative Integrated Ultrafiltration/Reverse Osmosis/Solid-Phase Extraction Procedure
title_sort fractionation of a procyanidin rich grape seed extract by a preparative integrated ultrafiltration reverse osmosis solid phase extraction procedure
topic grape seed extract
procyanidin fractionation
preparative ultrafiltration
reverse osmosis
preparative solid-phase extraction
url https://www.mdpi.com/2077-0375/15/3/92
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