Chiral separation of a basic drug with two chiral centers by electrokinetic chromatography for its pharmaceutical development

A chiral method using capillary electrophoresis was developed for the separation of the four stereoisomers of a new chiral substance currently undergoing drug development as single enantiomer. After the selection of highly sulfated beta-CD as chiral selector, an exhaustive study on the influence of...

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Detalles Bibliográficos
Autores: Martínez Girón, Ana Belén, Marina Alegre, María Luisa|||0000-0002-5583-1624, Crego Navazo, Antonio Luis|||0000-0002-4083-5294
Tipo de recurso: artículo
Fecha de publicación:2016
País:España
Institución:Universidad de Alcalá (UAH)
Repositorio:e_Buah Biblioteca Digital Universidad de Alcalá
Idioma:inglés
OAI Identifier:oai:ebuah.uah.es:10017/48188
Acceso en línea:http://hdl.handle.net/10017/48188
https://dx.doi.org/10.1016/j.chroma.2016.08.041
Access Level:acceso abierto
Palabra clave:Chiral drug
Enantiomeric purity
Chiral stability
Electrokinetic chromatography with cyclodextrins
Química
Chemistry
Descripción
Sumario:A chiral method using capillary electrophoresis was developed for the separation of the four stereoisomers of a new chiral substance currently undergoing drug development as single enantiomer. After the selection of highly sulfated beta-CD as chiral selector, an exhaustive study on the influence of several experimental variables on the resolution was performed, being the substitution degree of the CD a very decisive factor. Run time and resolutions were about 20 min and higher than 2.0, respectively. The method was validated in terms of selectivity, linearity, accuracy, precision, and limits of detection and quantitation according to the requirements of the International Conference on Harmonisation for the determination of the chiral purity of a drug substance. The usefulness of the method was demonstrated in the control of stereoisomeric impurities in raw material as well as in the determination of the chiral stability of the drug in the solid state and in dosage forms used in safety assessment. Finally, the chiral method was used to investigate the possible in vivo inversion in biological samples. (C) 2016 Elsevier B.V. All rights reserved.