Headspace solid-phase micro-extraction and gas chromatography-ion trap tandem mass spectrometry method for butyltin analysis in sediments: Optimization and validation

• Tipo: Artigo em Revista Científica Internacional
• Data: 2007

Autores

Pedro N Carvalho (Autor) Outra; Luiz F Pinto (Autor) Outra; Clara C P Basto (Autor) FCUP; Teresa T S D Vasconcelos (Autor) Outra

Revista

Título: Microchemical Journal

Vol. 87

Páginas: 147-153

ISSN: 0026-265X

Editora: Elsevier

Indexação

ISI Web of Knowledge - 17 Citações

Scopus - 19 Citações

Classificação Científica

FOS: Ciências exactas e naturais > Química

Outras Informações

ID Authenticus: P-004-64G

DOI: 10.1016/j.microc.2007.07.003

Abstract (EN): In this work, headspace solid-phase micro-extraction (SPME) combined with gas chromatography-mass spectrometry (GC-MS) method for analysis of butyltin compounds in sediment samples was upgraded by the introduction of tandem mass spectrometry (MS/MS). Optimization and validation of this method based on an one step procedure, tetraethylborate in situ ethylation with simultaneous extraction by headspace SPME, combined with tandem mass spectrometry is described. A simple leaching/extraction step of mono-(M), di-(D) and tri-(T) butyltin (BT) compounds from the sediment is required as sample pre-treatment. The combination of the two techniques headspace SPME and MS/MS, led to very little matrix interference which permitted to attain limits of detection three or more orders of magnitude lower than those attained in previous methods: 0.3 pg g(-1) for MBT, 1 pg g(-1) for DBT and 0.4 pg g(-1) for TBT. Linear response range was from 0.02-1260 ng g(-1) for MBT, 0.07-1568 ng g(-1) for DBT and 0.04-2146 ng g(-1) for TBT and RSD < 15% was also obtained. The method was efficiently applied to a real sample sediment from Sado River estuary in Portugal, revealing the existence of BTs pollution, as the TBT level of 189 +/- 15 ng g(-1) was much higher than the maximum established as provisional ecotoxicological assessment criteria.

Idioma: Inglês

Tipo (Avaliação Docente): Científica

Nº de páginas: 7