Headspace solid-phase micro-extraction and gas chromatography-ion trap tandem mass spectrometry method for butyltin analysis in sediments: Optimization and validation |
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Authors: | Pedro N Carvalho Luiz F Pinto M Clara P Basto M Teresa SD Vasconcelos |
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Institution: | aFaculdade de Ciências, Universidade do Porto, R. Campo Alegre 687, 4169-007 Porto, Portugal;bCIMAR/CIIMAR, R. dos Bragas 289, 4050-123 Porto, Portugal |
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Abstract: | 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. |
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Keywords: | Butyltin compounds Headspace solid-phase microextraction Sediments Gas chromatography-tandem mass spectrometry |
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