Abstract
Organotin compounds (OTCs) are among the most toxic substances ever introduced to the environment by man. They are common pollutants in marine ecosystems, but are also present in the terrestrial environment, accumulated mainly in sewage sludge and landfill leachates. In investigations of the degradation and methylation processes of OTC in environmental samples, the use of enriched isotopic tracers represents a powerful analytical tool. Sn-enriched OTC are also necessary in application of the isotope dilution mass spectrometry technique for their accurate quantification. Since Sn-enriched monobutyltin (MBT), dibutyltin (DBT) and tributyltin (TBT) are not commercially available as single species, "in house" synthesis of individual butyltin-enriched species is necessary. In the present work, the preparation of the most toxic butyltin, namely TBT, was performed via a simple synthetic path, starting with bromination of metallic Sn, followed by butylation with butyl lithium. The tetrabutyltin (TeBT) formed was transformed to tributyltin chloride (TBTCl) using concentrated hydrochloric acid (HCl). The purity of the synthesized TBT was verified by speciation analysis using the techniques of gas chromatography coupled to inductively coupled plasma mass spectrometry (GC-ICP-MS) and nuclear magnetic resonance (NMR). The results showed that TBT had a purity of more than 97%. The remaining 3% corresponded to DBT. TBT was quantified by reverse isotope dilution GC-ICP-MS. The synthesis yield was around 60%. The advantage of this procedure over those previously reported lies in its possibility to be applied on a micro-scale (starting with 10mg of metallic Sn). This feature is of crucial importance, since enriched metallic Sn is extremely expensive. The procedure is simple and repeatable, and was successfully applied for the preparation of (117)Sn-enriched TBTCl from (117)Sn-enriched metal.
PMID: 24472491 [PubMed - as supplied by publisher]
[NMR paper] Use of (1)h-nmr std, waterlogsy and langmuir monolayer techniques for characterization of drug- zein protein complexes.
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Eur J Pharm Biopharm. 2013 Jul 24;
Authors: Sousa FF, Luzardo-Álvarez A, Blanco-Méndez J, Otero-Espinar FJ, Martín-Pastor M, Sandez Macho I
Abstract
Zein is a protein based natural biopolymer containing a large amount of nonpolar amino acids, which has shown the ability to form...
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Use of 1h-nmr std, waterlogsy and langmuir monolayer techniques for characterization of drug- zein protein complexes
Use of 1h-nmr std, waterlogsy and langmuir monolayer techniques for characterization of drug- zein protein complexes
Publication date: Available online 24 July 2013
Source:European Journal of Pharmaceutics and Biopharmaceutics</br>
Author(s): F.F.O. Sousa , A. Luzardo-Álvarez , J. Blanco-Méndez , F.J. Otero-Espinar , M. Martín-Pastor , I. Sandez Macho</br>
Zein is a protein based natural biopolymer containing a large amount of nonpolar amino acids, which has shown the ability to form aggregates and entrap solutes, such as drugs and amino acids to form stable...
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Linear Mode
