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dc.contributor.authorCastro Puyana, María 
dc.contributor.authorGarcía Ruiz, Carmen 
dc.contributor.authorCifuentes Gallego, Alejandro
dc.contributor.authorCrego Navazo, Antonio Luis 
dc.contributor.authorMarina Alegre, María Luisa 
dc.date.accessioned2008-02-27T14:01:14Z
dc.date.available2008-02-27T14:01:14Z
dc.date.issued2006
dc.identifier.bibliographicCitationJournal of Chromatography A, 2006, v. 1114, p. 170-177en
dc.identifier.issn0021-9673
dc.identifier.urihttp://hdl.handle.net/10017/1347
dc.description.abstracttrans-Ketoconazole was identified and quantified as impurity of cis-ketoconazole, an antifungal compound, by capillary zone electrophoresis–electrospray–mass spectrometry (CZE–ESI–MS). The chirality of this impurity was demonstrated separating their enantiomers by adding heptakis-(2,3,6-tri-O-methyl)-β-cyclodextrin to the separation buffer in capillary electrophoresis (CE) with UV detection. However, MS detection was hyphenated to the CE instrument for its identification. As both compounds are diastereomers, they have the same m/z values and are needed to be separated prior to the MS identification. A 0.4 M ammonium formate separation buffer at pH 3.0 enabled the separation of the impurity from cis-ketoconazole. Under these conditions, the optimization of ESI–MS parameters (composition and flow of the sheath–liquid, drying temperature, drying gas flow, and capillary potential) was carried out to obtain the best MS sensitivity. CZE–ESI–MS optimized conditions enabled the identification of trans-ketoconazole as impurity of cis-ketoconazole. In addition, the quantitation of this impurity was achieved in different samples: cis-ketoconazole standard and three different pharmaceutical formulations (two tablets and one syrup) containing this standard. In all cases, percentages higher than 2.0 were determined for the impurity. According to ICH guidelines, these values required the identification and quantitation of any impurity in drug substances and products.en
dc.description.sponsorshipAuthors thank the Ministry of Science and Technology (Spain) for the research project BQU2003-03638. Carmen García-Ruiz thanks the Ministry of Science and Technology for the Ramón y Cajal program (RYC-2003-001). María CastroPuyana thanks the University of Alcala for her pre-doctoral grant.en
dc.format.mimetypeapplication/pdfen
dc.language.isoengen
dc.publisherElsevieren
dc.rights(c) Elsevier, 2006en
dc.subjectCis-Ketoconazoleen
dc.subjectTrans-Ketoconazoleen
dc.subjectCE-MSen
dc.subjectImpurityen
dc.subjectPharmaceutical formulationsen
dc.titleIdentification and quantitation of cis-ketoconazole impurity by capillary zone electrophoresis-mass spectrometryen
dc.typeinfo:eu-repo/semantics/articleen
dc.subject.ecienciaCienciaes_ES
dc.subject.ecienciaQuímica analítica e industriales_ES
dc.subject.ecienciaScienceen
dc.subject.ecienciaChemistry, analytic and technicalen
dc.contributor.affiliationUniversidad de Alcalá. Departamento de Química Analítica e Ingeniería Química
dc.relation.publisherversionhttp://dx.doi.org/10.1016/j.chroma.2006.02.030
dc.type.versioninfo:eu-repo/semantics/publishedVersionen
dc.identifier.doi10.1016/j.chroma.2006.02.030
dc.relation.projectIDinfo:eu-repo/grantAgreement/MICYT//BQU2003-03638/ES/CROMATOGRAFÍA ELECTROCINÉTICA: UNA PODEROSA HERRAMIENTA PARA LA SEPARACIÓN ENANTIOMÉRICA DE COMPUESTOS QUIRALES CON APLICACIÓN A LA DETERMINACIÓN DE LA PUREZA ENANTIOMÉRICAes_ES
dc.relation.projectIDinfo:eu-repo/grantAgreement/MEC//RYC-2003-001/ES/RYC-2003-001/es_ES
dc.rights.accessRightsinfo:eu-repo/semantics/openAccessen


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