Abstract
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 SnI4 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 C18 column for isolating and purifying single species. The yields of pure MPhT, DPhT, and TPhT, each synthesized from isotope-enriched 118Sn metal, 122Sn metal, and 124Sn 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 °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 °C or 22 °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.
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Acknowledgments
Funding was from the Knut and Alice Wallenberg as well as the Kempe Foundations. Dong Nguyen Van thanks the Ministry of Education and Training, Vietnam. Wolfgang Frech and Solomon Tesfalidet thank the North Sweden Soil Remediation Center (EU Structural Funds and New Objective 1, Contract 113-12534-00).
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Nguyen Van, D., Muppala, S.R.K., Frech, W. et al. Preparation, preservation and application of pure isotope-enriched phenyltin species. Anal Bioanal Chem 386, 1505–1513 (2006). https://doi.org/10.1007/s00216-006-0695-8
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DOI: https://doi.org/10.1007/s00216-006-0695-8