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Optimisation and validation of an analytical methodology for selected pesticides in waters by solid-phase extraction and liquid chromatography with ion-trap mass spectrometry detection

Título
Optimisation and validation of an analytical methodology for selected pesticides in waters by solid-phase extraction and liquid chromatography with ion-trap mass spectrometry detection
Tipo
Artigo em Revista Científica Internacional
Ano
2010
Autores
Rita Araújo
(Autor)
Outra
A pessoa não pertence à instituição. A pessoa não pertence à instituição. A pessoa não pertence à instituição. Sem AUTHENTICUS Sem ORCID
Lúcia Santos
(Autor)
FEUP
Revista
Vol. 90 3
Páginas: 205-218
ISSN: 0306-7319
Editora: Taylor & Francis
Indexação
Publicação em ISI Proceedings ISI Proceedings
Publicação em ISI Web of Science ISI Web of Science
COMPENDEX
Classificação Científica
FOS: Ciências exactas e naturais > Química
Outras Informações
ID Authenticus: P-003-BC8
Abstract (EN): Multiresidue analytical methodologies are being developed for several classes of pesticides, using either GC or LC techniques coupled with MS detection. However, to reach ultra-low levels, as imposed by recent European Directives, specific extraction methods must be applied. This work intends to present the optimisation steps followed to implement a method to analyse pesticides of different families, as diuron, bentazone and cymoxanil. Among three types of SPE sorbents tested (EnviCarb, Easy and HR-P), the best results were achieved with HR-P. Concerning LC/MS with electrospray ionisation, the ionisation modes (negative and positive in a single run), the individual mass fragmentation, the parent ions for subsequent fragmentation, the needle voltage and the RF loading, the excitation amplitude, as well as the determination of optimal conditions for temperature of the drying gas and the pressure values for the drying and nebulisation gases, were optimised. As quantification method, attending the relatively low extracting recoveries, matrix-matched calibration was used, in order to achieve detection limits at ng L(-1) levels. However, because high uncertainties are achieved, it is proposed that the optimised direct injection in LC/MS is the best approach. In these conditions, analysis could be performed in less than 10 minutes and the limits of detection were 0.48, 0.13 and 4.26 mu g L(-1) for diuron, bentazone and cymoxanil, respectively.
Idioma: Inglês
Tipo (Avaliação Docente): Científica
Nº de páginas: 14
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