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Quantification of endocrine disruptors and pesticides in water by gas chromatography-tandem mass spectrometry. Method validation using weighted linear regression schemes

dc.contributor.authorMansilha, C.
dc.contributor.authorMelo, A.
dc.contributor.authorRebelo, H.
dc.contributor.authorFerreira, I.M.
dc.contributor.authorPinho, O.
dc.contributor.authorDomingues, V.
dc.contributor.authorPinho, C.
dc.contributor.authorGameiro, P.
dc.date.accessioned2011-09-19T11:46:45Z
dc.date.available2011-09-19T11:46:45Z
dc.date.issued2010-10-22
dc.description.abstractA multi-residue methodology based on a solid phase extraction followed by gas chromatography-tandem mass spectrometry was developed for trace analysis of 32 compounds in water matrices, including estrogens and several pesticides from different chemical families, some of them with endocrine disrupting properties. Matrix standard calibration solutions were prepared by adding known amounts of the analytes to a residue-free sample to compensate matrix-induced chromatographic response enhancement observed for certain pesticides. Validation was done mainly according to the International Conference on Harmonisation recommendations, as well as some European and American validation guidelines with specifications for pesticides analysis and/or GC-MS methodology. As the assumption of homoscedasticity was not met for analytical data, weighted least squares linear regression procedure was applied as a simple and effective way to counteract the greater influence of the greater concentrations on the fitted regression line, improving accuracy at the lower end of the calibration curve. The method was considered validated for 31 compounds after consistent evaluation of the key analytical parameters: specificity, linearity, limit of detection and quantification, range, precision, accuracy, extraction efficiency, stability and robustness.por
dc.identifier.citationJ Chromatogr A. 2010 Oct 22;1217(43):6681-91. Epub 2010 May 6por
dc.identifier.issn0021-9673
dc.identifier.otherdoi:10.1016/j.chroma.2010.05.005
dc.identifier.urihttp://hdl.handle.net/10400.18/192
dc.language.isoengpor
dc.peerreviewedyespor
dc.publisherElsevierpor
dc.relation.publisherversionhttp://www.sciencedirect.com/science/article/pii/S0021967310006291por
dc.subjectEndocrine disruptorspor
dc.subjectPesticidespor
dc.subjectGC–MSpor
dc.subjectWaterpor
dc.subjectWeighted linear regression schemespor
dc.subjectValidationpor
dc.subjectÁgua e Solopor
dc.titleQuantification of endocrine disruptors and pesticides in water by gas chromatography-tandem mass spectrometry. Method validation using weighted linear regression schemespor
dc.typejournal article
dspace.entity.typePublication
oaire.citation.endPage6691por
oaire.citation.startPage6681por
oaire.citation.titleJournal of Chromatography Apor
rcaap.rightsrestrictedAccesspor
rcaap.typearticlepor

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