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...
| Autores: | , , , , , , , , , , , |
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| 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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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 Sí |
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info:eu-repo/semantics/openAccess |
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openAccess |
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Elsevier |
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Elsevier |
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reponame:DIGITAL.CSIC. Repositorio Institucional del CSIC instname:Consejo Superior de Investigaciones Científicas (CSIC) |
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Consejo Superior de Investigaciones Científicas (CSIC) |
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DIGITAL.CSIC. Repositorio Institucional del CSIC |
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DIGITAL.CSIC. Repositorio Institucional del CSIC |
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