Preparation, preservation and application of pure isotope-enriched phenyltin species.
2006 (English)In: Analytical and Bioanalytical Chemistry, ISSN 1618-2642, E-ISSN 1618-2650, Vol. 386, no 5, 1505-1513 p.Article in journal (Refereed) Published
A method combining liquid/liquid extraction and chromatographic fractionation has been developed for the preparation of pure monophenyltin (MPhT), diphenyltin (DPhT), and triphenyltin (TPhT), synthesized from isotope-enriched Sn metal using phenylation of SnI(4) in diethylether (DEE) followed by quenching with HBr and water. After two successive extractions of the aqueous HBr phase with DEE, >99% of both DPhT and TPhT was recovered in the combined DEE phase and 94% of the MPhT remained in the aqueous phase. The MPhT in the aqueous phase was extracted into dichloromethane. The organic phases were vaporized and the PhTs were redissolved in MeOH/water/acetic acid/sodium acetate (59/30/6/8, v/v/v/w), which was also used as storing solution. Aliquots of the two solutions containing either DPhT and TPhT or MPhT were injected into a silica-based C(18) column for isolating and purifying single species. The yields of pure MPhT, DPhT, and TPhT, each synthesized from isotope-enriched (118)Sn metal, (122)Sn metal, and (124)Sn metal, were better than 99%. After chromatographic separation, the single phenyltin compounds were mixed to prepare a spike for multiple-isotope species-specific isotope dilution (MI-SSID). MI-SSID was successfully used to determine phenyltin compounds in the certified reference material, mussel tissue BCR CRM-477. At -20 degrees C, all of the fractionated phenyltin species were stable in the storage solution for at least 197 days. When these standards were stored at 4 degrees C or 22 degrees C, 4-6% of the DPhT and TPhT degraded within 27 days. The degradation of DPhT and TPhT increased with the ionic strength and acidity of the storage solution.
Place, publisher, year, edition, pages
Berlin: Springer , 2006. Vol. 386, no 5, 1505-1513 p.
Chemical Fractionation/methods, Chromatography; Gas/methods, Chromatography; High Pressure Liquid/methods, Gas Chromatography-Mass Spectrometry/methods, Isotopes, Organotin Compounds/analysis/chemical synthesis, Reproducibility of Results, Sensitivity and Specificity, Time Factors
IdentifiersURN: urn:nbn:se:umu:diva-11788DOI: 10.1007/s00216-006-0695-8PubMedID: 16937090OAI: oai:DiVA.org:umu-11788DiVA: diva2:151459