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Quantitative analysis of glyphosate, glufosinate and AMPA in irrigation water by in situ derivatization–dispersive liquid–liquid microextraction combined with UPLC-MS/MS

dc.contributor.authorPinto, Edgar
dc.contributor.authorSoares, António Gomes
dc.contributor.authorFerreira, Isabel M. P. L. V. O.
dc.date.accessioned2019-06-27T16:00:05Z
dc.date.available2020-05-02T00:30:29Z
dc.date.issued2018
dc.description.abstractA novel method was developed for the sensitive, cheap and fast quantitation of glyphosate, glufosinate and aminomethylphosphonic acid (AMPA) in irrigation water by in situ derivatization and dispersive liquid–liquid microextraction (DLLME) combined with ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Water samples were filtered with a 0.22 μm nylon filter, pH adjusted to 9 with ammonium bicarbonate and derivatized with fluorenylmethyloxycarbonyl chloride (FMOC-Cl). Afterwards, DLLME was applied to concentrate the compounds of interest, which were then analyzed by UPLC-MS/MS. The best results were obtained when acetone and dichloromethane were used as dispersive and extraction solvents, respectively. Two-level full factorial designs and a central composite design were applied to select the most appropriate derivatization and DLLME conditions. The method performance was evaluated according to the SANTE/11945/2015 guidelines and was linear in the 1.0 to 200 μg L−1 range for glyphosate, glufosinate and AMPA, with r2 ≥ 0.997 and individual residuals <13%. Repeatability (RSDr) and within-laboratory reproducibility (RSDwr) ranged from 2.7 to 9.1% and from 3.4 to 14.3%, respectively, and the trueness between 94.9 and 118.1%. The limits of detection were 0.35, 0.05 and 0.10 μg L−1 for glyphosate, glufosinate and AMPA, respectively and the limit of quantitation was 1.0 μg L−1 for all three compounds. The developed method was successfully applied to the analysis of irrigation water (surface and groundwater). No sign of the three compounds was detected in the groundwater samples but glyphosate was quantified in surface waters.pt_PT
dc.description.versioninfo:eu-repo/semantics/publishedVersionpt_PT
dc.identifier.doi10.1039/C7AY02722Bpt_PT
dc.identifier.urihttp://hdl.handle.net/10400.22/14134
dc.language.isoengpt_PT
dc.peerreviewedyespt_PT
dc.publisherRoyal Society of Chemistrypt_PT
dc.relation.publisherversionhttps://pubs.rsc.org/en/content/articlelanding/2018/AY/C7AY02722B#!divAbstractpt_PT
dc.subjectGlyphosatept_PT
dc.subjectDLLMEpt_PT
dc.subjectAMPApt_PT
dc.subjectglufosinatept_PT
dc.subjectUPLC-MS/MSpt_PT
dc.subjectderivatizationpt_PT
dc.titleQuantitative analysis of glyphosate, glufosinate and AMPA in irrigation water by in situ derivatization–dispersive liquid–liquid microextraction combined with UPLC-MS/MSpt_PT
dc.typejournal article
dspace.entity.typePublication
oaire.citation.endPage561pt_PT
oaire.citation.issue5pt_PT
oaire.citation.startPage554pt_PT
oaire.citation.titleAnalytical Methodspt_PT
oaire.citation.volume10pt_PT
person.familyNamePinto
person.givenNameEdgar
person.identifier.ciencia-id271F-B7DF-8FAB
person.identifier.orcid0000-0002-8021-4783
rcaap.rightsopenAccesspt_PT
rcaap.typearticlept_PT
relation.isAuthorOfPublicationeaf9fc86-1a1c-437f-adee-d28040aa7f2f
relation.isAuthorOfPublication.latestForDiscoveryeaf9fc86-1a1c-437f-adee-d28040aa7f2f

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