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A survey of the occurrence of ochratoxin A in Madeira wines based on a modified QuEChERS extraction procedure combined with liquid chromatography–triple quadrupole tandem mass spectrometry

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dc.contributor.authorFernandes, Paulo J.
dc.contributor.authorBarros, Nelson
dc.contributor.authorCâmara, José S.
dc.date.accessioned2019-07-18T14:20:23Z
dc.date.available2019-07-18T14:20:23Z
dc.date.issued2013
dc.description.abstractOver the past years, to ensure food safety, the European Union (EU) has adopted specific legislation concerning the control of mycotoxins residue levels in different kinds of food. In this study, a fast, selective and sensitive reversed-phased liquid chromatography with tandem mass spectrometry (LC–MS/MS) methodology was developed and validated for quantification of ochratoxin A (OTA) in Madeira wines. Sample extraction and purification were performed with a modified QuEChERS-based (quick, easy, cheap, effective, rugged, and safe) procedure. Firstly, the homogenized samples are extracted and partitioned using an organic solvent and salt solution. Then, the supernatant is further extracted and cleaned using a dispersive solid phase extraction (dSPE) technique. Finally clear wine extracts were concentrated under vacuum to near dryness and taken up into initial mobile phase. Careful optimization of the LC–MS/MS parameters was achieved in order to attain a fast separation with the best sensitivity. The detection was carried out on a triple–quadrupole tandem mass spectrometer (MS/MS) by electrospray ionization in positive ion mode (ESI+) with multiple reaction monitoring (MRM). MS/MS conditions were optimized in order to increase selectivity, selecting the corresponding product ions (precursor-to-fragment m/z 404 → 239; m/z 404 → m/z 358) for quantification and identification. The performance of the method was assessed and compared to the European Commission (EC) Regulations, by studying the selectivity and specificity, limit of detection (LOD), limit of quantification (LOQ), linear dynamic range, matrix effect, accuracy, precision, robustness/ruggedness and uncertainty. The validation was performed by analyzing recovery samples at four different spiked concentrations, 0.5, 1.0, 5.0 and 10.0 μg/kg, with four replicates (n = 4) at each concentration. Recoveries ranged from 87.2% to 102.6%, with relative standard deviations below 9% in all cases. The intra-day precision and inter-day precision, expressed as relative standard deviation, were lower than 7% and 14%, respectively. Matrix effects were observed by comparing the slope of matrix-matched standard calibration with that of solvent. Good linearity was achieved at the concentration levels of 0.50–22.5 μg/L. The LOQ and LOD, 0.4 and 0.1 μg/kg, respectively, at the signal-to-noise ratio (S/N) of 10 and 3, were lower than the concentration usually permitted by legislation in wines. The method was successfully applied to evaluate the occurrence of OTA in 30 Madeira wine samples. None of the analyzed samples exceeded the maximum permissible limit for wines (2.0 μg/kg) set by the EC, which confirms that the risk of OTA occurrence in Madeira wines is, as expected, is very low.pt_PT
dc.description.versioninfo:eu-repo/semantics/publishedVersionpt_PT
dc.identifier.citationFernandes, P. J., Barros, N., & Câmara, J. S. (2013). A survey of the occurrence of ochratoxin A in Madeira wines based on a modified QuEChERS extraction procedure combined with liquid chromatography–triple quadrupole tandem mass spectrometry. Food research international, 54(1), 293-301.pt_PT
dc.identifier.doi10.1016/j.foodres.2013.07.020pt_PT
dc.identifier.issn0963-9969
dc.identifier.urihttp://hdl.handle.net/10400.13/2482
dc.language.isoengpt_PT
dc.peerreviewedyespt_PT
dc.publisherElsevierpt_PT
dc.relationStrategic Project - UI 674 - 2011-2012
dc.subjectOchratoxin Apt_PT
dc.subjectWinept_PT
dc.subjectQuEChERSpt_PT
dc.subjectLC–ESI-MS/MSpt_PT
dc.subject.pt_PT
dc.subjectFaculdade de Ciências Exatas e da Engenhariapt_PT
dc.subjectCentro de Química da Madeira
dc.titleA survey of the occurrence of ochratoxin A in Madeira wines based on a modified QuEChERS extraction procedure combined with liquid chromatography–triple quadrupole tandem mass spectrometrypt_PT
dc.typejournal article
dspace.entity.typePublication
oaire.awardTitleStrategic Project - UI 674 - 2011-2012
oaire.awardURIinfo:eu-repo/grantAgreement/FCT/6817 - DCRRNI ID/PEst-OE%2FQUI%2FUI0674%2F2011/PT
oaire.citation.endPage301pt_PT
oaire.citation.startPage293pt_PT
oaire.citation.titleFood Research Internationalpt_PT
oaire.citation.volume54(1)pt_PT
oaire.fundingStream6817 - DCRRNI ID
person.familyNameCâmara
person.givenNameJosé
person.identifierG-3003-2013
person.identifier.ciencia-id481C-08CE-90E5
person.identifier.orcid0000-0003-1965-3151
person.identifier.scopus-author-id10140393000
project.funder.identifierhttp://doi.org/10.13039/501100001871
project.funder.nameFundação para a Ciência e a Tecnologia
rcaap.rightsrestrictedAccesspt_PT
rcaap.typearticlept_PT
relation.isAuthorOfPublicatione10d78be-e547-4d25-92b5-06a997ed78da
relation.isAuthorOfPublication.latestForDiscoverye10d78be-e547-4d25-92b5-06a997ed78da
relation.isProjectOfPublication595c1582-33c0-493a-8ab3-37d2811536d9
relation.isProjectOfPublication.latestForDiscovery595c1582-33c0-493a-8ab3-37d2811536d9

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