Development, validation and evaluation of an analytical method for the determination of monomeric and oligomeric procyanidins in apple extracts

There is a lack of data for individual oligomeric procyanidins in apples and apple extracts. Our aim was to develop, validate and evaluate an analytical method for the separation, identification and quantification of monomeric and oligomeric flavanols in apple extracts. To achieve this, we prepared...

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Autores: Hollands, Wendy J., Voorspoels, Stefan, Jacobs, Griet, Aaby, Kjersti, Meisland, Ane, García-Villalba, Rocío, Tomás Barberán, Francisco, Piskula, Mariusz K., Mawson, Deborah, Vovk, Irena, Needs, Paul W., Kroon, Paul A.
Tipo de recurso: artículo
Estado:Versión publicada
Fecha de publicación:2017
País:España
Institución:Consejo Superior de Investigaciones Científicas (CSIC)
Repositorio:DIGITAL.CSIC. Repositorio Institucional del CSIC
OAI Identifier:oai:digital.csic.es:10261/152147
Acceso en línea:http://hdl.handle.net/10261/152147
Access Level:acceso abierto
Palabra clave:Flavanols flavan-3-ols
Tannins
Polyphenols
Phenolics
HPLC
Inter-laboratory evaluation
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spelling Development, validation and evaluation of an analytical method for the determination of monomeric and oligomeric procyanidins in apple extractsHollands, Wendy J.Voorspoels, StefanJacobs, GrietAaby, KjerstiMeisland, AneGarcía-Villalba, RocíoTomás Barberán, FranciscoPiskula, Mariusz K.Mawson, DeborahVovk, IrenaNeeds, Paul W.Kroon, Paul A.Flavanols flavan-3-olsTanninsPolyphenolsPhenolicsHPLCInter-laboratory evaluationThere is a lack of data for individual oligomeric procyanidins in apples and apple extracts. Our aim was to develop, validate and evaluate an analytical method for the separation, identification and quantification of monomeric and oligomeric flavanols in apple extracts. To achieve this, we prepared two types of flavanol extracts from freeze-dried apples; one was an epicatechin-rich extract containing ∼30% (w/w) monomeric (−)-epicatechin which also contained oligomeric procyanidins (Extract A), the second was an oligomeric procyanidin-rich extract depleted of epicatechin (Extract B). The parameters considered for method optimisation were HPLC columns and conditions, sample heating, mass of extract and dilution volumes. The performance characteristics considered for method validation included standard linearity, method sensitivity, precision and trueness. Eight laboratories participated in the method evaluation. Chromatographic separation of the analytes was best achieved utilizing a Hilic column with a binary mobile phase consisting of acidic acetonitrile and acidic aqueous methanol. The final method showed linearity for epicatechin in the range 5–100 μg/mL with a correlation co-efficient >0.999. Intra-day and inter-day precision of the analytes ranged from 2 to 6% and 2 to 13% respectively. Up to dp3, trueness of the method was >95% but decreased with increasing dp. Within laboratory precision showed RSD values <5 and 10% for monomers and oligomers, respectively. Between laboratory precision was 4 and 15% (Extract A) and 7 and 30% (Extract B) for monomers and oligomers, respectively. An analytical method for the separation, identification and quantification of procyanidins in an apple extract was developed, validated and assessed. The results of the inter-laboratory evaluation indicate that the method is reliable and reproducible.This research has received funding from the European Community’s Seventh Framework Programme (FP7 under agreement no. 312090, project BACCHUS) and the Biotechnology and Biological Sciences Research Council (UK) through an Institute Strategic Programme Grant (‘Food and Health’; Grant No: BB/J004545/1) to the Institute of Food Research.Peer reviewedElsevierEuropean CommissionBiotechnology and Biological Sciences Research Council (UK)Consejo Superior de Investigaciones Científicas [https://ror.org/02gfc7t72]201720172017info:eu-repo/semantics/articlehttp://purl.org/coar/resource_type/c_6501Publisher's versioninfo:eu-repo/semantics/publishedVersionhttp://hdl.handle.net/10261/152147reponame:DIGITAL.CSIC. Repositorio Institucional del CSICinstname:Consejo Superior de Investigaciones Científicas (CSIC)Inglés#PLACEHOLDER_PARENT_METADATA_VALUE#info:eu-repo/grantAgreement/EC/FP7/312090https://doi.org/10.1016/j.chroma.2017.03.030Síinfo:eu-repo/semantics/openAccessoai:digital.csic.es:10261/1521472026-05-22T06:33:51Z
dc.title.none.fl_str_mv Development, validation and evaluation of an analytical method for the determination of monomeric and oligomeric procyanidins in apple extracts
title Development, validation and evaluation of an analytical method for the determination of monomeric and oligomeric procyanidins in apple extracts
spellingShingle Development, validation and evaluation of an analytical method for the determination of monomeric and oligomeric procyanidins in apple extracts
Hollands, Wendy J.
Flavanols flavan-3-ols
Tannins
Polyphenols
Phenolics
HPLC
Inter-laboratory evaluation
title_short Development, validation and evaluation of an analytical method for the determination of monomeric and oligomeric procyanidins in apple extracts
title_full Development, validation and evaluation of an analytical method for the determination of monomeric and oligomeric procyanidins in apple extracts
title_fullStr Development, validation and evaluation of an analytical method for the determination of monomeric and oligomeric procyanidins in apple extracts
title_full_unstemmed Development, validation and evaluation of an analytical method for the determination of monomeric and oligomeric procyanidins in apple extracts
title_sort Development, validation and evaluation of an analytical method for the determination of monomeric and oligomeric procyanidins in apple extracts
dc.creator.none.fl_str_mv Hollands, Wendy J.
Voorspoels, Stefan
Jacobs, Griet
Aaby, Kjersti
Meisland, Ane
García-Villalba, Rocío
Tomás Barberán, Francisco
Piskula, Mariusz K.
Mawson, Deborah
Vovk, Irena
Needs, Paul W.
Kroon, Paul A.
author Hollands, Wendy J.
author_facet Hollands, Wendy J.
Voorspoels, Stefan
Jacobs, Griet
Aaby, Kjersti
Meisland, Ane
García-Villalba, Rocío
Tomás Barberán, Francisco
Piskula, Mariusz K.
Mawson, Deborah
Vovk, Irena
Needs, Paul W.
Kroon, Paul A.
author_role author
author2 Voorspoels, Stefan
Jacobs, Griet
Aaby, Kjersti
Meisland, Ane
García-Villalba, Rocío
Tomás Barberán, Francisco
Piskula, Mariusz K.
Mawson, Deborah
Vovk, Irena
Needs, Paul W.
Kroon, Paul A.
author2_role author
author
author
author
author
author
author
author
author
author
author
dc.contributor.none.fl_str_mv European Commission
Biotechnology and Biological Sciences Research Council (UK)
Consejo Superior de Investigaciones Científicas [https://ror.org/02gfc7t72]
dc.subject.none.fl_str_mv Flavanols flavan-3-ols
Tannins
Polyphenols
Phenolics
HPLC
Inter-laboratory evaluation
topic Flavanols flavan-3-ols
Tannins
Polyphenols
Phenolics
HPLC
Inter-laboratory evaluation
description There is a lack of data for individual oligomeric procyanidins in apples and apple extracts. Our aim was to develop, validate and evaluate an analytical method for the separation, identification and quantification of monomeric and oligomeric flavanols in apple extracts. To achieve this, we prepared two types of flavanol extracts from freeze-dried apples; one was an epicatechin-rich extract containing ∼30% (w/w) monomeric (−)-epicatechin which also contained oligomeric procyanidins (Extract A), the second was an oligomeric procyanidin-rich extract depleted of epicatechin (Extract B). The parameters considered for method optimisation were HPLC columns and conditions, sample heating, mass of extract and dilution volumes. The performance characteristics considered for method validation included standard linearity, method sensitivity, precision and trueness. Eight laboratories participated in the method evaluation. Chromatographic separation of the analytes was best achieved utilizing a Hilic column with a binary mobile phase consisting of acidic acetonitrile and acidic aqueous methanol. The final method showed linearity for epicatechin in the range 5–100 μg/mL with a correlation co-efficient >0.999. Intra-day and inter-day precision of the analytes ranged from 2 to 6% and 2 to 13% respectively. Up to dp3, trueness of the method was >95% but decreased with increasing dp. Within laboratory precision showed RSD values <5 and 10% for monomers and oligomers, respectively. Between laboratory precision was 4 and 15% (Extract A) and 7 and 30% (Extract B) for monomers and oligomers, respectively. An analytical method for the separation, identification and quantification of procyanidins in an apple extract was developed, validated and assessed. The results of the inter-laboratory evaluation indicate that the method is reliable and reproducible.
publishDate 2017
dc.date.none.fl_str_mv 2017
2017
2017
dc.type.none.fl_str_mv info:eu-repo/semantics/article
http://purl.org/coar/resource_type/c_6501
Publisher's version
info:eu-repo/semantics/publishedVersion
format article
status_str publishedVersion
dc.identifier.none.fl_str_mv http://hdl.handle.net/10261/152147
url http://hdl.handle.net/10261/152147
dc.language.none.fl_str_mv Inglés
language_invalid_str_mv Inglés
dc.relation.none.fl_str_mv #PLACEHOLDER_PARENT_METADATA_VALUE#
info:eu-repo/grantAgreement/EC/FP7/312090
https://doi.org/10.1016/j.chroma.2017.03.030

dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
eu_rights_str_mv openAccess
dc.publisher.none.fl_str_mv Elsevier
publisher.none.fl_str_mv Elsevier
dc.source.none.fl_str_mv reponame:DIGITAL.CSIC. Repositorio Institucional del CSIC
instname:Consejo Superior de Investigaciones Científicas (CSIC)
instname_str Consejo Superior de Investigaciones Científicas (CSIC)
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collection DIGITAL.CSIC. Repositorio Institucional del CSIC
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