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Optimisation and validation of a HS-SPME-GC-IT/MS method for analysis of carbonyl volatile compounds as biomarkers in human urine: Application in a pilot study to discriminate individuals with smoking habits

2016Journal article Restricted access
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dc.contributor.authorCalejo, Isabel
dc.contributor.authorMoreira, Nathalie
dc.contributor.authorAraújo, Ana Margarida
dc.contributor.authorCarvalho, Márcia
dc.contributor.authorBastos, Maria de Lourdes
dc.contributor.authorPinho, Paula Guedes de
dc.date.accessioned2017-10-13T07:49:54Z
dc.date.available2017-10-13T07:49:54Z
dc.date.issued2016
dc.description.abstractA new and simple analytical approach consisting of an automated headspace solid-phase microextraction (HS-SPME) sampler coupled to gas chromatography-ion trap/mass spectrometry detection (GC–IT/MS) with a prior derivatization step with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA) was developed to detect volatile carbonyl metabolites with low molecular weights in human urine. A central composite design (CCD) was used to optimise the PFBHA concentration and extraction conditions that affect the efficiency of the SPME procedure. With a sample volume of 1 mL, optimal conditions were achieved by adding 300 mg/L of PFBHA and allowing the sample to equilibrate for 6 min at 62 °C and then extracting the samples for 51 min at the same temperature, using a divinylbenzene/polydimethylsiloxane (DVB/PDMS) fibre. The method allowed the simultaneous identification and quantification of 44 carbonyl compounds consisting of aldehydes, dialdehydes, heterocyclic aldehydes and ketones. The method was validated with regards to the linearity, inter- and intra-day precision and accuracy. The detection limits ranged from 0.009 to 0.942 ng/mL, except for 4-hydroxy-2-nonenal (15 ng/mL), and the quantification limits varied from 0.029 to 1.66 ng/mL, except for butanal (2.78 ng/mL), 2-butanone (2.67 ng/mL), 4-heptanone (3.14 ng/mL) and 4-hydroxy-2-nonenal (50.0 ng/mL). The method accuracy was satisfactory, with recoveries ranging from 90 to 107%. The proof of applicability of the methodology was performed in a pilot target analysis of urine samples obtained from 18 healthy smokers and 18 healthy non-smokers (control group). Chemometric supervised analysis was performed using the volatile patterns acquired for these samples and clearly showed the potential of the volatile carbonyl profiles to discriminate urine from smoker and non-smoker subjects. 5-Methyl-2-furfural (p<0.0001), 2-methylpropanal, nonanal and 2-methylbutanal (p<0.05) were identified as potentially useful biomarkers to identify smoking habits.pt_PT
dc.description.versioninfo:eu-repo/semantics/publishedVersionpt_PT
dc.identifier.citationCALEJO, Isabel; MOREIRA, Nathalie; ARAÚJO, Ana Margarida; CARVALHO, Márcia; BASTOS, Maria de Lourdes; PINHO, Paula Guedes de - Optimisation and validation of a HS-SPME-GC-IT/MS method for analysis of carbonyl volatile compounds as biomarkers in human urine: Application in a pilot study to discriminate individuals with smoking habits. Talanta. ISSN: 0039-9140. Vol. 148 (2016), p. 486-493pt_PT
dc.identifier.doi10.1016/j.talanta.2015.09.070pt_PT
dc.identifier.eid84947081354
dc.identifier.pmid26653476
dc.identifier.urihttp://hdl.handle.net/10400.14/23064
dc.identifier.wos000366786400061
dc.language.isoengpt_PT
dc.peerreviewedyespt_PT
dc.relationPest-OE/EQB/ LA0006/2013pt_PT
dc.relationSULPHUR COMPOUNDS IN GRAPES AND WINES FROM PORTUGUESE VARIETIES: CHEMICAL AND ORGANOLEPTIC PROFILE CHARACTERIZATION; BIOAVAILABILITY AND BIOLOGICAL ACTIVITY STUDIES
dc.subjectHS-SPME–GC–IT/MS methodpt_PT
dc.subjectCentralpt_PT
dc.subjectCompositept_PT
dc.subjectDesign(CCD)pt_PT
dc.subjectCarbonyl compoundspt_PT
dc.subjectUrinary biomarkerspt_PT
dc.subjectSmoking habitspt_PT
dc.titleOptimisation and validation of a HS-SPME-GC-IT/MS method for analysis of carbonyl volatile compounds as biomarkers in human urine: Application in a pilot study to discriminate individuals with smoking habitspt_PT
dc.typejournal article
dspace.entity.typePublication
oaire.awardTitleSULPHUR COMPOUNDS IN GRAPES AND WINES FROM PORTUGUESE VARIETIES: CHEMICAL AND ORGANOLEPTIC PROFILE CHARACTERIZATION; BIOAVAILABILITY AND BIOLOGICAL ACTIVITY STUDIES
oaire.awardURIinfo:eu-repo/grantAgreement/FCT/3599-PPCDT/PTDC%2FAGR-ALI%2F121062%2F2010/PT
oaire.awardURIinfo:eu-repo/grantAgreement/FCT/FARH/SFRH%2FBPD%2F63851%2F2009/PT
oaire.citation.endPage493
oaire.citation.startPage486
oaire.citation.titleTalantapt_PT
oaire.citation.volume148
oaire.fundingStream3599-PPCDT
oaire.fundingStreamFARH
person.familyNameCalejo
person.familyNameMoreira
person.familyNameAraújo
person.familyNameCarvalho
person.familyNameBastos
person.familyNameGuedes de Pinho
person.givenNameIsabel
person.givenNameNathalie
person.givenNameAna Margarida
person.givenNameMarcia
person.givenNameMaria de Lourdes
person.givenNamePaula
person.identifier1180817
person.identifier2017111
person.identifier392870
person.identifier.ciencia-id1A1F-B26C-15CC
person.identifier.ciencia-idE91D-B71A-E36F
person.identifier.ciencia-id8B10-171E-E63E
person.identifier.ciencia-idC31F-AAC1-24D5
person.identifier.ciencia-id2510-1418-EF48
person.identifier.orcid0000-0002-6015-0655
person.identifier.orcid0000-0002-4862-7510
person.identifier.orcid0000-0002-4073-2121
person.identifier.orcid0000-0001-9884-4751
person.identifier.orcid0000-0001-9895-503X
person.identifier.orcid0000-0002-7395-5700
person.identifier.ridS-3103-2016
person.identifier.ridD-5498-2013
person.identifier.ridT-3699-2017
person.identifier.ridD-5999-2013
person.identifier.ridD-8588-2013
person.identifier.scopus-author-id56960478900
person.identifier.scopus-author-id56191198700
person.identifier.scopus-author-id7201413997
person.identifier.scopus-author-id25822248900
person.identifier.scopus-author-id6504448214
project.funder.identifierhttp://doi.org/10.13039/501100001871
project.funder.identifierhttp://doi.org/10.13039/501100001871
project.funder.nameFundação para a Ciência e a Tecnologia
project.funder.nameFundação para a Ciência e a Tecnologia
rcaap.rightsrestrictedAccesspt_PT
rcaap.typearticlept_PT
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