Repository logo
 
Publication

Definitive screening designs and latent variable modelling for the optimization of solid phase microextraction (SPME): case study-quantification of volatile fatty acids in wines

2018Journal article Open access
Simple item page
dc.contributor.authorPereira, Ana C.
dc.contributor.authorReis, Marco S.
dc.contributor.authorLeça, João M.
dc.contributor.authorRodrigues, Pedro M.
dc.contributor.authorMarques, José C.
dc.date.accessioned2021-10-13T14:01:30Z
dc.date.available2021-10-13T14:01:30Z
dc.date.issued2018
dc.description.abstractIn the present study, we apply the recently proposed Definitive Screening Designs (DSD) to optimize HS-SPME extraction in order to analyze volatile fatty acids (VFA) present in wine samples. This is the first attempt to apply this new class of designs to one of the most well-known and widely applied extraction techniques. The latent structure of the responses is also explored for defining the optimal extraction conditions. DSD is a new screening design with the potential to significantly reduce the number of experiments required to estimate the model pa rameters and to establish the optimum operation conditions. Therefore, there is an obvious interest in assessing the benefits of DSD in practice. In this work, this design framework is applied to the simultaneous optimization of seven extraction parameters (responses). Both qualitative and quantitative extraction parameters are considered, in order to test the flexibility of DSD designs: a two-level qualitative variable, the fiber coating, and six quanti tative variables, namely the pre-incubation time, the extraction time and temperature, the headspace/sample volume, the effect of agitation during extraction and the influence of the ethanol content (sample dilution). Optimization of analytes' chromatographic responses was carried out both individually (response by response) and altogether, by modelling the responses in the latent variable space (i.e., explicitly considering their under lying correlation structure). In the end, a consensus analysis of all perspectives was considered in the definition of the overall optimal extraction conditions for the quantification of VFA in fortified wines. The solution found was to use a DVB/Car/PDMS fiber, 10 mL of samples in 20 mL vial, 40 min of extraction at 40 C. The analysis also revealed that the factors incubation time, agitation and sample dilution do not play a significant role in explaining the variability of extraction parameters. Therefore, they were set to the most convenient levels. The methodology followed was thoroughly validated and the following figures of merit were obtained: good linearity (R2 > 0.999, for all compounds), high sensitivity (LOD and LOQ are close or below the values found in literature), recoveries of approximately 100% and suitable precision (repeatability and reproducibility lower than 7.21% and 8.61%, respectively). Finally, the optimized methodology was tested in practice. Several wine samples were analyzed and the odor activity value calculated to facilitate the identification of their importance as odor active compounds in different aged fortified wines. This work demonstrates the benefits of using DSD and latent variable modelling for the optimization of analytical techniques, contributing to the implementation of rigorous, systematic and more efficient optimization protocols.pt_PT
dc.description.versioninfo:eu-repo/semantics/publishedVersionpt_PT
dc.identifier.citationPereira, A. C., Reis, M. S., Leça, J. M., Rodrigues, P. M., & Marques, J. C. (2018). Definitive screening designs and latent variable modelling for the optimization of solid phase microextraction (SPME): case study-quantification of volatile fatty acids in wines. Chemometrics and Intelligent Laboratory Systems, 179, 73-81. https://doi.org/10.1016/j.chemolab.2018.06.010pt_PT
dc.identifier.doi10.1016/j.chemolab.2018.06.010pt_PT
dc.identifier.urihttp://hdl.handle.net/10400.13/3723
dc.language.isoengpt_PT
dc.peerreviewedyespt_PT
dc.publisherElsevierpt_PT
dc.rights.urihttp://creativecommons.org/licenses/by-nc-nd/4.0/pt_PT
dc.subjectDefinitive Screening Designspt_PT
dc.subjectPrincipal component analysispt_PT
dc.subjectHS-SPMEpt_PT
dc.subjectOptimizationpt_PT
dc.subjectVolatile fatty acidspt_PT
dc.subjectFortified winespt_PT
dc.subjectWeighted least squarespt_PT
dc.subject.pt_PT
dc.subjectFaculdade de Ciências da Vidapt_PT
dc.subjectFaculdade de Ciências Exatas e da Engenhariapt_PT
dc.titleDefinitive screening designs and latent variable modelling for the optimization of solid phase microextraction (SPME): case study-quantification of volatile fatty acids in winespt_PT
dc.typejournal article
dspace.entity.typePublication
oaire.citation.endPage81pt_PT
oaire.citation.startPage73pt_PT
oaire.citation.titleChemometrics and Intelligent Laboratory Systemspt_PT
oaire.citation.volume179pt_PT
person.familyNamePereira
person.familyNameReis
person.familyNameLeça
person.familyNameMarques
person.givenNameAna Cristina
person.givenNameMarco
person.givenNameJoão Micael
person.givenNameJose C
person.identifier1374847
person.identifier1083569
person.identifier.ciencia-id251D-B696-A3D1
person.identifier.ciencia-id9817-7687-05DC
person.identifier.ciencia-id6213-EB73-1A9F
person.identifier.ciencia-id1713-6DA1-A551
person.identifier.orcid0000-0003-3097-7704
person.identifier.orcid0000-0002-4997-8865
person.identifier.orcid0000-0003-1704-6745
person.identifier.orcid0000-0002-4832-4341
person.identifier.ridA-7681-2015
person.identifier.ridG-7266-2019
person.identifier.ridF-3014-2010
person.identifier.scopus-author-id56483357000
person.identifier.scopus-author-id9273948800
person.identifier.scopus-author-id55979990800
person.identifier.scopus-author-id7203033313
rcaap.rightsopenAccesspt_PT
rcaap.typearticlept_PT
relation.isAuthorOfPublication6ba13ec2-560d-4e9a-aa6d-0ec57000dcbc
relation.isAuthorOfPublication26d14a5e-49af-4fc1-80c4-6945a582a809
relation.isAuthorOfPublicationda166c1d-bdcc-4b21-afd0-4b3e5906b3ea
relation.isAuthorOfPublication08f4685f-b917-410a-b153-59911ff7d75e
relation.isAuthorOfPublication.latestForDiscovery26d14a5e-49af-4fc1-80c4-6945a582a809

Files

Original bundle
Now showing 1 - 1 of 1
Thumbnail Image
Name:
Definitive Screening Designs and latent variable modelling for the optimization of solid phase microextraction (SPME).pdf
Size:
511.16 KB
Format:
Adobe Portable Document Format
Download

Collections

Artigos em revistas internacionais