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Enantioselective determination of thyroxine enantiomers by ligand-exchange CE with UV absorbance and ICP-MS detection

Autor(es) y otros:
Kang, JianzhenAutoridad Uniovi; Kutscher, Daniel JurgenAutoridad Uniovi; Montes Bayón, MaríaAutoridad Uniovi; Blanco González, ElisaAutoridad Uniovi; Sanz Medel, AlfredoAutoridad Uniovi
Palabra(s) clave:

Ce-Icp-Ms; Chiral Speciation; Enantioselective Ce; Ligand-Exchange; Thyroxine Enantiomers

Fecha de publicación:
2009
Versión del editor:
http://dx.doi.org/10.1002/elps.200800731
Citación:
Electrophoresis, 30(10), p. 1774-1782 (2009); doi:10.1002/elps.200800731
Descripción física:
p. 1774-1782
Resumen:

A simple CE method has been developed for the separation and determination of thyroxine (T4) enantiomers in pharmaceutical formulations. The method was based on ligand-exchange mechanism using a Cu(II)/L-proline complex as chiral selector. The effects of different parameters affecting separation such as chiral selector concentration, organic additive, buffer pH and temperature were investigated. A baseline separation of the two enantiomers was obtained at a Cu(II)/L-proline ratio of 1:8 in a borate buffer (15 mmol/L, pH 9.6) containing 10% v/v acetonitrile. Under the optimized conditions, precision linearity range and detection limits of the developed enantioselective CE method were evaluated and compared using two different detection systems: conventional UV detection at 226 nm and iodine (127I)specific detection (“chiral speciation”) with ICP-MS. Both methodologies show adequate analytical performance characteristics with detection limits around 0.30 μg/mL for each enantiomer of T4. Finally, a levothroid pharmaceutical formulation sample was successfully analyzed using both developed methods CE-UV and CE-ICP-MS.

A simple CE method has been developed for the separation and determination of thyroxine (T4) enantiomers in pharmaceutical formulations. The method was based on ligand-exchange mechanism using a Cu(II)/L-proline complex as chiral selector. The effects of different parameters affecting separation such as chiral selector concentration, organic additive, buffer pH and temperature were investigated. A baseline separation of the two enantiomers was obtained at a Cu(II)/L-proline ratio of 1:8 in a borate buffer (15 mmol/L, pH 9.6) containing 10% v/v acetonitrile. Under the optimized conditions, precision linearity range and detection limits of the developed enantioselective CE method were evaluated and compared using two different detection systems: conventional UV detection at 226 nm and iodine (127I)specific detection (“chiral speciation”) with ICP-MS. Both methodologies show adequate analytical performance characteristics with detection limits around 0.30 μg/mL for each enantiomer of T4. Finally, a levothroid pharmaceutical formulation sample was successfully analyzed using both developed methods CE-UV and CE-ICP-MS.

URI:
http://hdl.handle.net/10651/7528
ISSN:
0173-0835
Identificador local:

20090604

DOI:
10.1002/elps.200800731
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