Extent of the influence of phosphate buffer and ionic liquids on the reduction of the silanol effect in a C18 stationary phase
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Otros documentos de la autoría: Carda-Broch, Samuel; García-Álvarez Coque, M. C.; Ruiz Ángel, M. J.
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https://doi.org/10.1016/j.chroma.2017.05.061 |
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Título
Extent of the influence of phosphate buffer and ionic liquids on the reduction of the silanol effect in a C18 stationary phaseFecha de publicación
2017-06Editor
ElsevierCita bibliográfica
CARDA-BROCH, S.; GARCÍA-ALVAREZ-COQUE, M. C.; RUIZ-ANGEL, M. J. Extent of the influence of phosphate buffer and ionic liquids on the reduction of the silanol effect in a C18 stationary phase. Journal of Chromatography A, 2017.Tipo de documento
info:eu-repo/semantics/articleVersión de la editorial
https://www.sciencedirect.com/science/article/pii/S0021967317308002Versión
info:eu-repo/semantics/publishedVersionPalabras clave / Materias
Resumen
The presence of anionic free silanols in the silica-based stationary phases gives rise to broad and asymmetrical peaks when cationic basic compounds are chromatographed using hydro-organic mobile phases. The addition ... [+]
The presence of anionic free silanols in the silica-based stationary phases gives rise to broad and asymmetrical peaks when cationic basic compounds are chromatographed using hydro-organic mobile phases. The addition to the mobile phase of a reagent with ionic character prevents the access of analytes to the free silanols, improving the peak shape. The silanol activity can be affected by the buffer concentration and mobile phase pH, factors that are not always considered sufficiently in the literature. In this work, the chromatographic behaviour of three basic β‐adrenoceptor antagonists (acebutolol, nadolol and timolol), using mobile phases containing acetonitrile, was examined at different phosphate buffer concentrations (5–50 mM) and mobile phase pH (2–8), in the absence and presence of three imidazolium-based ionic liquids (1‐ethyl-, 1‐butyl- and 1-hexyl-3-methylimidazolium chloride). All factors were evaluated through both the retention and peak shape. The imidazolium cations can block the access of cationic analytes through electrostatic interaction with the anionic silanols, or association with the alkyl chains bound to the stationary phase. In previous reports, the protection mechanism was demonstrated to be directly related to the cation size. The studies in this work reveal that the effectiveness of the mobile phase additive as silanol blocker also depends on the concentration of the buffer anion and the protonation degree of the silanols on the stationary phase. Increasing amounts of phosphate at low pH give rise to increasing retention times. Also, the peak shape is improved, which indicates the influence of phosphate on blocking the activity of free silanols. However, the benefits obtained by the combined effect of buffering the mobile phase at low pH and the use of a bulky additive are lost at pH > 6. [-]
Proyecto de investigación
Ministry of Economy and Competitiveness (MINECO, Spain) and FEDER funds [Project CTQ2016–75644-P]; Direcció General d’Universitat, Investigació i Ciència (Generalitat Valenciana, Spain) [Project PROMETEO/2016/128]Derechos de acceso
© 2017 Elsevier B.V. All rights reserved.
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