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Rapid and sensitive methodology for determination of ethyl carbamate in fortified wines using microextraction by packed sorbent and gas chromatography with mass spectrometric detection

2014Journal article Open access
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dc.contributor.authorLeça, João M.
dc.contributor.authorPereira, Vanda
dc.contributor.authorPereira, Ana C.
dc.contributor.authorMarques, José C.
dc.date.accessioned2021-10-14T10:51:45Z
dc.date.available2021-10-14T10:51:45Z
dc.date.issued2014
dc.description.abstractThis work presents a new methodology to quantify ethyl carbamate (EC) in fortified wines. The presented approach combines the microextraction by packed sorbent (MEPS), using a hand-held automated ana lytical syringe, with one-dimensional gas chromatography coupled with mass spectrometry detection (GC–MS). The performance of different MEPS sorbent materials was tested, namely SIL, C2, C8, C18, and M1. Also, several extraction solvents and the matrix effect were evaluated. Experimental data showed that C8 and dichloromethane were the best sorbent/solvent pair to extract EC. Concerning solvent and sample volumes optimization used in MEPS extraction an experimental design (DoE) was carried out. The best extraction yield was achieved passing 300 L of sample and 100 L of dichloromethane. The method validation was performed using a matrix-matched calibration using both sweet and dry fortified wines, to minimize the matrix effect. The proposed methodology presented good linearity (R2 = 0.9999) and high sensitivity, with quite low limits of detection (LOD) and quantification (LOQ), 1.5 g L−1 and 4.5 g L−1, respectively. The recoveries varied between 97% and 106%, while the method precision (repeatability and reproducibility) was lower than 7%. The applicability of the methodology was confirmed through the analysis of 16 fortified wines, with values ranging between 7.3 and 206 g L−1. All chromatograms showed good peak resolution, confirming its selectivity. The developed MEPS/GC–MS methodology arises as an importanttoolto quantify EC in fortified wines, combining efficiency and effectiveness, with simpler, faster and affordable analytical procedures that provide great sensitivity without using sophisticated and expensive equipment.pt_PT
dc.description.versioninfo:eu-repo/semantics/publishedVersionpt_PT
dc.identifier.citationLeça, J. M., Pereira, V., Pereira, A. C., & Marques, J. C. (2014). Rapid and sensitive methodology for determination of ethyl carbamate in fortified wines using microextraction by packed sorbent and gas chromatography with mass spectrometric detection. Analytica chimica acta, 811, 29-35. https://doi.org/10.1016/j.aca.2013.12.018pt_PT
dc.identifier.doi10.1016/j.aca.2013.12.018pt_PT
dc.identifier.urihttp://hdl.handle.net/10400.13/3728
dc.language.isoengpt_PT
dc.peerreviewedyespt_PT
dc.publisherElsevierpt_PT
dc.rights.urihttp://creativecommons.org/licenses/by-nc-nd/4.0/pt_PT
dc.subjectEthyl carbamatept_PT
dc.subjectWinespt_PT
dc.subjectMicroextraction by packed sorbentpt_PT
dc.subjectGas chromatography–mass spectrometric detectionpt_PT
dc.subject.pt_PT
dc.subjectEscola Superior de Tecnologias e Gestãopt_PT
dc.subjectFaculdade de Ciências da Vidapt_PT
dc.subjectFaculdade de Ciências Exatas e da Engenhariapt_PT
dc.titleRapid and sensitive methodology for determination of ethyl carbamate in fortified wines using microextraction by packed sorbent and gas chromatography with mass spectrometric detectionpt_PT
dc.typejournal article
dspace.entity.typePublication
oaire.citation.endPage35pt_PT
oaire.citation.startPage29pt_PT
oaire.citation.titleAnalytica Chimica Actapt_PT
oaire.citation.volume811pt_PT
person.familyNameLeça
person.familyNamePereira
person.familyNamePereira
person.familyNameMarques
person.givenNameJoão Micael
person.givenNameVanda
person.givenNameAna Cristina
person.givenNameJose C
person.identifier1083569
person.identifier41146
person.identifier.ciencia-id6213-EB73-1A9F
person.identifier.ciencia-id0115-071E-87E8
person.identifier.ciencia-id251D-B696-A3D1
person.identifier.ciencia-id1713-6DA1-A551
person.identifier.orcid0000-0003-1704-6745
person.identifier.orcid0000-0003-0772-8953
person.identifier.orcid0000-0003-3097-7704
person.identifier.orcid0000-0002-4832-4341
person.identifier.ridJ-8697-2013
person.identifier.ridA-7681-2015
person.identifier.ridF-3014-2010
person.identifier.scopus-author-id55979990800
person.identifier.scopus-author-id36857887700
person.identifier.scopus-author-id56483357000
person.identifier.scopus-author-id7203033313
rcaap.rightsopenAccesspt_PT
rcaap.typearticlept_PT
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