Repository logo
 
Publication

Optimal design of experiments applied to headspace solid phase microextraction for the quantification of vicinal diketones in beer through gas chromatography-mass spectrometric detection

2015Journal article Open access
Simple item page
dc.contributor.authorLeça, João M.
dc.contributor.authorPereira, Ana C.
dc.contributor.authorVieira, Ana C.
dc.contributor.authorReis, Marco S.
dc.contributor.authorMarques, José C.
dc.date.accessioned2021-10-14T10:23:34Z
dc.date.available2021-10-14T10:23:34Z
dc.date.issued2015
dc.description.abstractVicinal diketones, namely diacetyl (DC) and pentanedione (PN), are compounds naturally found in beer that play a key role in the definition of its aroma. In lager beer, they are responsible for off-flavors (buttery flavor) and therefore their presence and quantification is of paramount importance to beer producers. Aiming at developing an accurate quantitative monitoring scheme to follow these off-flavor compounds during beer production and in the final product, the head space solid-phase microextraction (HS-SPME) analytical procedure was tuned through experiments planned in an optimal way and the final settings were fully validated. Optimal design of experiments (O-DOE) is a computational, statistically oriented approach for designing experiences that are most informative according to a well-defined criterion. This methodology was applied for HS-SPME optimization, leading to the following optimal extraction conditions for the quantification of VDK: use a CAR/PDMS fiber, 5 ml of samples in 20 ml vial, 5 min of pre-incubation time followed by 25 min of extraction at 30 C, with agitation. The validation of the final analytical methodology was performed using a matrix-matched calibration, in order to mini mize matrix effects. The following key features were obtained: linearity (R2 > 0.999, both for diacetyl and 2,3-pentanedione), high sensitivity (LOD of 0.92 mg L 1 and 2.80 mg L 1 , and LOQ of 3.30 mg L 1 and 10.01 mg L 1 , for diacetyl and 2,3-pentanedione, respectively), recoveries of approximately 100% and suitable precision (repeatability and reproducibility lower than 3% and 7.5%, respectively). The applicability of the methodology was fully confirmed through an independent analysis of several beer samples, with analyte concentrations ranging from 4 to 200 g L 1pt_PT
dc.description.versioninfo:eu-repo/semantics/publishedVersionpt_PT
dc.identifier.citationLeça, J. M., Pereira, A. C., Vieira, A. C., Reis, M. S., & Marques, J. C. (2015). Optimal design of experiments applied to headspace solid phase microextraction for the quantification of vicinal diketones in beer through gas chromatography-mass spectrometric detection. Analytica chimica acta, 887, 101-110. https://doi.org/10.1016/j.aca.2015.06.044pt_PT
dc.identifier.doi10.1016/j.aca.2015.06.044pt_PT
dc.identifier.urihttp://hdl.handle.net/10400.13/3727
dc.language.isoengpt_PT
dc.peerreviewedyespt_PT
dc.publisherElsevierpt_PT
dc.rights.urihttp://creativecommons.org/licenses/by-nc-nd/4.0/pt_PT
dc.subjectVicinal diketonespt_PT
dc.subjectHeadspace solid phase microextractionpt_PT
dc.subjectOptimizationpt_PT
dc.subjectOptimal design of experimentspt_PT
dc.subject.pt_PT
dc.subjectFaculdade de Ciências da Vidapt_PT
dc.subjectEscola Superior de Tecnologias e Gestãopt_PT
dc.subjectFaculdade de Ciências Exatas e da Engenhariapt_PT
dc.titleOptimal design of experiments applied to headspace solid phase microextraction for the quantification of vicinal diketones in beer through gas chromatography-mass spectrometric detectionpt_PT
dc.typejournal article
dspace.entity.typePublication
oaire.citation.endPage110pt_PT
oaire.citation.startPage101pt_PT
oaire.citation.titleAnalytica Chimica Actapt_PT
oaire.citation.volume887pt_PT
person.familyNameLeça
person.familyNamePereira
person.familyNameLeal Vieira
person.familyNameReis
person.familyNameMarques
person.givenNameJoão Micael
person.givenNameAna Cristina
person.givenNameAna Carolina
person.givenNameMarco
person.givenNameJose C
person.identifier1083569
person.identifier1374847
person.identifier.ciencia-id6213-EB73-1A9F
person.identifier.ciencia-id251D-B696-A3D1
person.identifier.ciencia-id1F18-D56D-A988
person.identifier.ciencia-id9817-7687-05DC
person.identifier.ciencia-id1713-6DA1-A551
person.identifier.orcid0000-0003-1704-6745
person.identifier.orcid0000-0003-3097-7704
person.identifier.orcid0000-0003-3701-9648
person.identifier.orcid0000-0002-4997-8865
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-id55979990800
person.identifier.scopus-author-id56483357000
person.identifier.scopus-author-id9273948800
person.identifier.scopus-author-id7203033313
rcaap.rightsopenAccesspt_PT
rcaap.typearticlept_PT
relation.isAuthorOfPublicationda166c1d-bdcc-4b21-afd0-4b3e5906b3ea
relation.isAuthorOfPublication6ba13ec2-560d-4e9a-aa6d-0ec57000dcbc
relation.isAuthorOfPublication6d7bdaef-995b-4ba2-90f5-53a7e675af2c
relation.isAuthorOfPublication26d14a5e-49af-4fc1-80c4-6945a582a809
relation.isAuthorOfPublication08f4685f-b917-410a-b153-59911ff7d75e
relation.isAuthorOfPublication.latestForDiscovery6ba13ec2-560d-4e9a-aa6d-0ec57000dcbc

Files

Original bundle
Now showing 1 - 1 of 1
Thumbnail Image
Name:
Optimal design of experiments applied to headspace solid phase microextraction for the quantification of vicinal diketones in beer through gas chromatography-mass spectrometric detection.pdf
Size:
1.48 MB
Format:
Adobe Portable Document Format
Download

Collections

Artigos em revistas internacionais