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High-throughput analytical strategy based on modified QuEChERS extraction and dispersive solid-phase extraction clean-up followed by liquid chromatography-triple-quadrupole tandem mass spectrometry for quantification of multiclass mycotoxins in cereals

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dc.contributor.authorFernandes, Paulo J.
dc.contributor.authorBarros, Nelson
dc.contributor.authorSanto, José L.
dc.contributor.authorCâmara, José S.
dc.date.accessioned2019-07-22T15:09:50Z
dc.date.available2019-07-22T15:09:50Z
dc.date.issued2014
dc.description.abstractA simple, reliable, efficient, selective and sensitive QuEChERS-based (quick, easy, cheap, effective, rugged and safe) sample preparation strategy, involving an initial partitioning step using acidified acetonitrile (ACN), MgSO4, NaCl and citrate buffer salts, combined with dispersive solid-phase extraction (d-SPE) clean-up, is proposed for the simultaneous multiclass mycotoxins quantification, including aflatoxins, ochratoxins, fumonisins, trichothecenes and zearalenone, in cereals. The final clear extracts were concentrated under vacuum to near dryness and taken-up with the initial mobile phase (MeOH:H2O;70:30, v/v) previous to reversed-phase liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) analysis. Careful optimization of the LC-ESI-MS/MS parameters was achieved in order to attain a fast separation and increased sensitivity. The detection was carried out on a triple-quadrupole tandem mass spectrometry (MS/MS) by electrospray ionization in positive ion mode (ESI+) with multiple reaction monitoring (MRM). Tandem MS conditions were optimised in order to increase selectivity, selecting the best transitions (parent ion to quantifier and qualifier ions) for quantification and identification. The performance of the method was assessed and compared to European Commission (EC) Regulations, by studying the selectivity, specificity, limits of detection (LOD) and quantification (LOQ), linear dynamic range (LDR), matrix effect, accuracy, precision, and uncertainty. Good linearity (r 2 > 0.9713) was achieved for all mycotoxins investigated, and LODs (S/N = 3) and LOQs (S/N = 10) were below the tolerance levels of mycotoxins set by EC. Recoveries of the extraction process, obtained with different spiked concentrations, ranged from 72.9 to 120.6 %, with relative standard deviations (RSD) lower than 23.0 %. Only in 6 % of all combinations did the RSD values exceed 15 %. Matrix effects were observed by comparing the slope of matrix-matched standard calibration with that of the solvent. The developed method was applied to evaluate the co-occurrence of multiclass mycotoxins in cereals collected at the importation points and consumer habitations at Madeira Island. Samples collected at importation points (15 wheat samples, 4 maize samples and 2 rice samples) showed the presence of DON in three wheat samples, and FB1 and HT-2 in one wheat sample. Three maize samples were detected with FB1 (two samples) and AFG2 (one sample) whereas one rice sample was detected with ZEN. The results revealed the absence of target mycotoxins on the rice samples collected at consumer habitations. None of the studied cereal samples exceeded the maximum permissible limits or indicative levels set by the EC which means that the particular Madeira Island subtropical climate conditions do not represent a major risk for cereal contamination, taking into account the investigated mycotoxins.pt_PT
dc.description.versioninfo:eu-repo/semantics/publishedVersionpt_PT
dc.identifier.citationFernandes, P. J., Barros, N., Santo, J. L., & Câmara, J. S. (2015). High-throughput analytical strategy based on modified QuEChERS extraction and dispersive solid-phase extraction clean-up followed by liquid chromatography-triple-quadrupole tandem mass spectrometry for quantification of multiclass mycotoxins in cereals. Food analytical methods, 8(4), 841-856.pt_PT
dc.identifier.doi10.1007/s12161-014-9947-ypt_PT
dc.identifier.issn1936-9751
dc.identifier.urihttp://hdl.handle.net/10400.13/2497
dc.language.isoengpt_PT
dc.peerreviewedyespt_PT
dc.publisherSpringerpt_PT
dc.subjectQuEChERSpt_PT
dc.subjectd-SPEpt_PT
dc.subjectLC-ESI-MS/MSpt_PT
dc.subjectMycotoxinspt_PT
dc.subjectCerealspt_PT
dc.subject.pt_PT
dc.subjectFaculdade de Ciências Exatas e da Engenhariapt_PT
dc.subjectCentro de Química da Madeira
dc.titleHigh-throughput analytical strategy based on modified QuEChERS extraction and dispersive solid-phase extraction clean-up followed by liquid chromatography-triple-quadrupole tandem mass spectrometry for quantification of multiclass mycotoxins in cerealspt_PT
dc.typejournal article
dspace.entity.typePublication
oaire.awardURIinfo:eu-repo/grantAgreement/FCT/5876/PEst-OE%2FQUI%2FUI0674%2F2014/PT
oaire.citation.endPage856pt_PT
oaire.citation.startPage841pt_PT
oaire.citation.titleFood Analytical Methodspt_PT
oaire.citation.volume8(4)pt_PT
oaire.fundingStream5876
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.isProjectOfPublicationec6bb904-b852-4300-a638-266ee44773f0
relation.isProjectOfPublication.latestForDiscoveryec6bb904-b852-4300-a638-266ee44773f0

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