Enantiomeric separation of colchicine and lacosamide by nano-LC. Quantitative analysis in pharmaceutical formulations

A chiral analytical methodology was developed by nano-liquid chromatography (nano-LC) enabling the enantiomeric separation of two chiral drugs, lacosamide (novel antiepileptic drug) and colchicine (antiuremic drug), commercialized as pure enantiomers. A capillary column lab-packed with an amylose tr...

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Detalhes bibliográficos
Autores: Marina Alegre, María Luisa|||0000-0002-5583-1624, García González, María Ángeles|||0000-0001-6292-8232, Casado Navas, Natalia, Jiang, Z.
Formato: artículo
Fecha de publicación:2020
País:España
Recursos:Universidad de Alcalá (UAH)
Repositorio:e_Buah Biblioteca Digital Universidad de Alcalá
Idioma:inglés
OAI Identifier:oai:ebuah.uah.es:10017/46907
Acesso em linha:http://hdl.handle.net/10017/46907
https://dx.doi.org/10.3390/separations7040055
Access Level:acceso abierto
Palavra-chave:amylose-based stationary phase
chiral separation
enantiomers
colchicine
lacosamide
nano-LC
pharmaceutical formulation
drug analysis
chiral impurities
quality control
Química
Chemistry
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spelling Enantiomeric separation of colchicine and lacosamide by nano-LC. Quantitative analysis in pharmaceutical formulationsMarina Alegre, María Luisa|||0000-0002-5583-1624García González, María Ángeles|||0000-0001-6292-8232Casado Navas, NataliaJiang, Z.amylose-based stationary phasechiral separationenantiomerscolchicinelacosamidenano-LCpharmaceutical formulationdrug analysischiral impuritiesquality controlQuímicaChemistryA chiral analytical methodology was developed by nano-liquid chromatography (nano-LC) enabling the enantiomeric separation of two chiral drugs, lacosamide (novel antiepileptic drug) and colchicine (antiuremic drug), commercialized as pure enantiomers. A capillary column lab-packed with an amylose tris(3,5-dimethylphenylcarbamate) chiral stationary phase was used in a lab-assembled nano-LC system. Lacosamide and colchicine enantiomers were separated in less than 8.0 and 9.0 min, respectively, with resolution values of 1.6 and 2.3, using 20 nL of sample and 1.8 mu L of mobile phase per analysis. The analytical characteristics of the proposed methodology were evaluated according to the International Council for Harmonisation (ICH) guidelines, showing good analytical performance with good recoveries (97-98% and 100-103%) and precision values (relative standard deviation (RSD) <10.5 and <3.0%) for lacosamide and colchicine enantiomers, respectively. LODs were 1.7 and 2.0 mu g/mL for (S)- and (R)-lacosamide, respectively, and 1.0 mu g/mL for both colchicine enantiomers. Additionally, the developed methodology enabled to detect a 0.1% of the enantiomeric impurities, fulfilling the ICH regulation requirements. The method was applied to the determination of lacosamide and colchicine enantiomers in different pharmaceutical formulations to ensure their quality control. The content of the enantiomeric impurities was below a 0.1% and the amount of (R)-lacosamide and (S)-colchicine agreed with their labeled contents.Universidad de AlcaláMinisterio de Economía, Industria y Competitividad20202020-10-16journal articlehttp://purl.org/coar/resource_type/c_6501NAhttp://purl.org/coar/version/c_be7fb7dd8ff6fe43info:eu-repo/semantics/articleapplication/pdfhttp://hdl.handle.net/10017/46907https://dx.doi.org/10.3390/separations7040055reponame:e_Buah Biblioteca Digital Universidad de Alcaláinstname:Universidad de Alcalá (UAH)InglésengUAH Not available CCG19%2FCC-068 Desarrollo de nuevas metodologías para el análisis y evaluación de la actividadMinisterio de Economía y Competitividad http://dx.doi.org/10.13039/501100003329 Not available CTQ2013-48740-P Metodologías avanzadas para análisis quiral mediante técnicas microseparativas. Búsqueda de biomarcadores en sistemas enantioselectivosMinisterio de Economía y Competitividad http://dx.doi.org/10.13039/501100003329 Not available CTQ2016-76368 Nnuevos nanoaditivos para separación quiral por electrofóresis capilar. Aplicación a la determinación de biomarcadoresopen accesshttp://purl.org/coar/access_right/c_abf2Attribution-NonCommercial-ShareAlike 4.0 Internationalhttp://creativecommons.org/licenses/by-nc-sa/4.0/info:eu-repo/semantics/openAccessoai:ebuah.uah.es:10017/469072026-06-18T11:13:07Z
dc.title.none.fl_str_mv Enantiomeric separation of colchicine and lacosamide by nano-LC. Quantitative analysis in pharmaceutical formulations
title Enantiomeric separation of colchicine and lacosamide by nano-LC. Quantitative analysis in pharmaceutical formulations
spellingShingle Enantiomeric separation of colchicine and lacosamide by nano-LC. Quantitative analysis in pharmaceutical formulations
Marina Alegre, María Luisa|||0000-0002-5583-1624
amylose-based stationary phase
chiral separation
enantiomers
colchicine
lacosamide
nano-LC
pharmaceutical formulation
drug analysis
chiral impurities
quality control
Química
Chemistry
title_short Enantiomeric separation of colchicine and lacosamide by nano-LC. Quantitative analysis in pharmaceutical formulations
title_full Enantiomeric separation of colchicine and lacosamide by nano-LC. Quantitative analysis in pharmaceutical formulations
title_fullStr Enantiomeric separation of colchicine and lacosamide by nano-LC. Quantitative analysis in pharmaceutical formulations
title_full_unstemmed Enantiomeric separation of colchicine and lacosamide by nano-LC. Quantitative analysis in pharmaceutical formulations
title_sort Enantiomeric separation of colchicine and lacosamide by nano-LC. Quantitative analysis in pharmaceutical formulations
dc.creator.none.fl_str_mv Marina Alegre, María Luisa|||0000-0002-5583-1624
García González, María Ángeles|||0000-0001-6292-8232
Casado Navas, Natalia
Jiang, Z.
author Marina Alegre, María Luisa|||0000-0002-5583-1624
author_facet Marina Alegre, María Luisa|||0000-0002-5583-1624
García González, María Ángeles|||0000-0001-6292-8232
Casado Navas, Natalia
Jiang, Z.
author_role author
author2 García González, María Ángeles|||0000-0001-6292-8232
Casado Navas, Natalia
Jiang, Z.
author2_role author
author
author
dc.subject.none.fl_str_mv amylose-based stationary phase
chiral separation
enantiomers
colchicine
lacosamide
nano-LC
pharmaceutical formulation
drug analysis
chiral impurities
quality control
Química
Chemistry
topic amylose-based stationary phase
chiral separation
enantiomers
colchicine
lacosamide
nano-LC
pharmaceutical formulation
drug analysis
chiral impurities
quality control
Química
Chemistry
description A chiral analytical methodology was developed by nano-liquid chromatography (nano-LC) enabling the enantiomeric separation of two chiral drugs, lacosamide (novel antiepileptic drug) and colchicine (antiuremic drug), commercialized as pure enantiomers. A capillary column lab-packed with an amylose tris(3,5-dimethylphenylcarbamate) chiral stationary phase was used in a lab-assembled nano-LC system. Lacosamide and colchicine enantiomers were separated in less than 8.0 and 9.0 min, respectively, with resolution values of 1.6 and 2.3, using 20 nL of sample and 1.8 mu L of mobile phase per analysis. The analytical characteristics of the proposed methodology were evaluated according to the International Council for Harmonisation (ICH) guidelines, showing good analytical performance with good recoveries (97-98% and 100-103%) and precision values (relative standard deviation (RSD) <10.5 and <3.0%) for lacosamide and colchicine enantiomers, respectively. LODs were 1.7 and 2.0 mu g/mL for (S)- and (R)-lacosamide, respectively, and 1.0 mu g/mL for both colchicine enantiomers. Additionally, the developed methodology enabled to detect a 0.1% of the enantiomeric impurities, fulfilling the ICH regulation requirements. The method was applied to the determination of lacosamide and colchicine enantiomers in different pharmaceutical formulations to ensure their quality control. The content of the enantiomeric impurities was below a 0.1% and the amount of (R)-lacosamide and (S)-colchicine agreed with their labeled contents.
publishDate 2020
dc.date.none.fl_str_mv 2020
2020-10-16
dc.type.none.fl_str_mv journal article
http://purl.org/coar/resource_type/c_6501
NA
http://purl.org/coar/version/c_be7fb7dd8ff6fe43
dc.type.openaire.fl_str_mv info:eu-repo/semantics/article
format article
dc.identifier.none.fl_str_mv http://hdl.handle.net/10017/46907
https://dx.doi.org/10.3390/separations7040055
url http://hdl.handle.net/10017/46907
https://dx.doi.org/10.3390/separations7040055
dc.language.none.fl_str_mv Inglés
eng
language_invalid_str_mv Inglés
language eng
dc.relation.none.fl_str_mv UAH Not available CCG19%2FCC-068 Desarrollo de nuevas metodologías para el análisis y evaluación de la actividad
Ministerio de Economía y Competitividad http://dx.doi.org/10.13039/501100003329 Not available CTQ2013-48740-P Metodologías avanzadas para análisis quiral mediante técnicas microseparativas. Búsqueda de biomarcadores en sistemas enantioselectivos
Ministerio de Economía y Competitividad http://dx.doi.org/10.13039/501100003329 Not available CTQ2016-76368 Nnuevos nanoaditivos para separación quiral por electrofóresis capilar. Aplicación a la determinación de biomarcadores
dc.rights.none.fl_str_mv open access
http://purl.org/coar/access_right/c_abf2
Attribution-NonCommercial-ShareAlike 4.0 International
http://creativecommons.org/licenses/by-nc-sa/4.0/
dc.rights.openaire.fl_str_mv info:eu-repo/semantics/openAccess
rights_invalid_str_mv open access
http://purl.org/coar/access_right/c_abf2
Attribution-NonCommercial-ShareAlike 4.0 International
http://creativecommons.org/licenses/by-nc-sa/4.0/
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv application/pdf
dc.source.none.fl_str_mv reponame:e_Buah Biblioteca Digital Universidad de Alcalá
instname:Universidad de Alcalá (UAH)
instname_str Universidad de Alcalá (UAH)
reponame_str e_Buah Biblioteca Digital Universidad de Alcalá
collection e_Buah Biblioteca Digital Universidad de Alcalá
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