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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.authorGuedes de Pinho, Paula
dc.date.accessioned2021-07-02T11:59:45Z
dc.date.available2021-07-02T11:59:45Z
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.doi10.1016/j.talanta.2015.09.070pt_PT
dc.identifier.issn0039-9140
dc.identifier.urihttp://hdl.handle.net/10284/10024
dc.language.isoengpt_PT
dc.peerreviewedyespt_PT
dc.publisherElsevierpt_PT
dc.relationThis work was supported by National Funds from FCT (Fundação para a Ciência e a Tecnologia) through project Pest-OE/EQB/ LA0006/2013, Wine Metrics: Revealing the Volatile Molecular Feature Responsible for the Wine Like Aroma a Critical Task Toward the Wine. Quality Definition - PTDC/AGR-ALI/121062/2010 and postgraduate fellowship ref. SFRH/BPD/63851/2009pt_PT
dc.subjectHS-SPME–GC–IT/MS methodpt_PT
dc.subjectCentral Composite Design (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.citation.endPage493pt_PT
oaire.citation.startPage486pt_PT
oaire.citation.titleTalantapt_PT
oaire.citation.volume148pt_PT
person.familyNameCarvalho
person.givenNameMarcia
person.identifier2017111
person.identifier.ciencia-id8B10-171E-E63E
person.identifier.orcid0000-0001-9884-4751
person.identifier.ridD-5999-2013
person.identifier.scopus-author-id7201413997
rcaap.rightsclosedAccesspt_PT
rcaap.typearticlept_PT
relation.isAuthorOfPublication3837b828-ba57-47f7-a811-cce65e4922c6
relation.isAuthorOfPublication.latestForDiscovery3837b828-ba57-47f7-a811-cce65e4922c6

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