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Development of a novel microextraction by packed sorbent-based approach followed by ultrahigh pressure liquid chromatography as a powerful technique for quantification phenolic constituents of biological interest in wines

2012-03Journal article Open access
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dc.contributor.authorGonçalves, João
dc.contributor.authorMendes, Berta Rodrigues
dc.contributor.authorSilva, Catarina L.
dc.contributor.authorCâmara, José S.
dc.date.accessioned2015-12-10T11:27:44Z
dc.date.available2015-12-10T11:27:44Z
dc.date.issued2012-03
dc.description.abstractA novel analytical approach, based on a miniaturized extraction technique, the microextraction by packed sorbent (MEPS), followed by ultrahigh pressure liquid chromatography (UHPLC) separation combined with a photodiode array (PDA) detection, has been developed and validated for the quantitative determination of sixteen biologically active phenolic constituents of wine. In addition to performing routine experiments to establish the validity of the assay to internationally accepted criteria (linearity, sensitivity, selectivity, precision, accuracy), experiments are included to assess the effect of the important experimental parameters on the MEPS performance such as the type of sorbent material (C2, C8, C18, SIL, and M1), number of extraction cycles (extract-discard), elution volume, sample volume, and ethanol content, were studied. The optimal conditions of MEPS extraction were obtained using C8 sorbent and small sample volumes (250 μL) in five extraction cycle and in a short time period (about 5 min for the entire sample preparation step). The wine bioactive phenolics were eluted by 250 μL of the mixture containing 95% methanol and 5% water, and the separation was carried out on a HSS T3 analytical column (100 mm × 2.1 mm, 1.8 μm particle size) using a binary mobile phase composed of aqueous 0.1% formic acid (eluent A) and methanol (eluent B) in the gradient elution mode (10 min of total analysis). The method gave satisfactory results in terms of linearity with r2-values > 0.9986 within the established concentration range. The LOD varied from 85 ng mL−1 (ferulic acid) to 0.32 μg mL−1 ((+)-catechin), whereas the LOQ values from 0.028 μg mL−1 (ferulic acid) to 1.08 μg mL−1 ((+)-catechin). Typical recoveries ranged between 81.1 and 99.6% for red wines and between 77.1 and 99.3% for white wines, with relative standard deviations (RSD) no larger than 10%. The extraction yields of the MEPSC8/UHPLC–PDA methodology were found between 78.1 (syringic acid) and 99.6% (o-coumaric acid) for red wines and between 76.2 and 99.1% for white wines. The inter-day precision, expressed as the relative standard deviation (RSD%), varied between 0.2% (p-coumaric and o-coumaric acids) and 7.5% (gentisic acid) while the intra-day precision between 0.2% (o-coumaric and cinnamic acids) and 4.7% (gallic acid and (−)-epicatechin). On the basis of analytical validation, it is shown that the MEPSC8/UHPLC–PDA methodology proves to be an improved, reliable, and ultra-fast approach for wine bioactive phenolics analysis, because of its capability for determining simultaneously in a single chromatographic run several bioactive metabolites with high sensitivity, selectivity and resolving power within only 10 min. Preliminary studies have been carried out on 34 real whole wine samples, in order to assess the performance of the described procedure. The new approach offers decreased sample preparation and analysis time, and moreover is cheaper, more environmentally friendly and easier to perform as compared to traditional methodologies.pt_PT
dc.identifier.citationGonçalves, J., Mendes, B., Silva, C. L., & Câmara, J. S. (2012). Development of a novel microextraction by packed sorbent-based approach followed by ultrahigh pressure liquid chromatography as a powerful technique for quantification phenolic constituents of biological interest in wines. Journal of Chromatography A, 1229, 13-23.pt_PT
dc.identifier.doi10.1016/j.chroma.2012.01.023pt_PT
dc.identifier.urihttp://hdl.handle.net/10400.13/946
dc.language.isoengpt_PT
dc.peerreviewedyespt_PT
dc.publisherElsevierpt_PT
dc.subjectWinespt_PT
dc.subjectBioactive compoundspt_PT
dc.subjectMicroextraction by packed sorbent (MEPS)pt_PT
dc.subjectUltra high pressure liquid chromatographypt_PT
dc.subject.pt_PT
dc.subjectFaculdade de Ciências Exatas e da Engenhariapt_PT
dc.subjectCentro de Química da Madeira
dc.titleDevelopment of a novel microextraction by packed sorbent-based approach followed by ultrahigh pressure liquid chromatography as a powerful technique for quantification phenolic constituents of biological interest in winespt_PT
dc.typejournal article
dspace.entity.typePublication
oaire.citation.endPage23pt_PT
oaire.citation.startPage13pt_PT
oaire.citation.titleJournal of Chromatography Apt_PT
oaire.citation.volume1229pt_PT
person.familyNameGonçalves
person.familyNameSousa Luís
person.familyNameCâmara
person.givenNameJoão
person.givenNameCatarina Grace
person.givenNameJosé
person.identifierC-1300-2019
person.identifierG-3003-2013
person.identifier.ciencia-id8C14-3188-9E44
person.identifier.ciencia-id9813-3B88-BA8D
person.identifier.ciencia-id481C-08CE-90E5
person.identifier.orcid0000-0002-1265-6686
person.identifier.orcid0000-0002-3018-3165
person.identifier.orcid0000-0003-1965-3151
person.identifier.ridC-1348-2019
person.identifier.scopus-author-id52163735200
person.identifier.scopus-author-id57194492726
person.identifier.scopus-author-id10140393000
rcaap.rightsopenAccesspt_PT
rcaap.typearticlept_PT
relation.isAuthorOfPublication7971c475-3f08-4462-96b1-79e96c9615a4
relation.isAuthorOfPublication2853e6b6-0fb5-454c-aedb-05528b76c484
relation.isAuthorOfPublicatione10d78be-e547-4d25-92b5-06a997ed78da
relation.isAuthorOfPublication.latestForDiscovery7971c475-3f08-4462-96b1-79e96c9615a4

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