Elaboration de phases stationnaires originales pour la Chromatographie Liquide Haute Performance : Synthèse, caractérisation, et évaluation des propriétés chromatographiques des colonnes.

Abstract : To achieve high throughput or high efficiency in chromatography, one can think about High-Temperature or Ultra-High-Performance Liquid Chromatography. Nevertheless, such efficient approaches require a dedicated instrumentation that is costly. Since a few years, the core-shell technology (i. E. Superficially porous particles) is of crucial interest as it combines high efficiency with low-pressure, allowing to work with conventional HPLC instrument. The development of different stationary phase chemistries give access to orthogonal and/or complementary separation mechanisms that are useful for difficult separation or to increase the peak capacity for instance with a second dimension. Developments are still in progress to offer a wide range of core-shell stationary phases to meet the needs of analytical scientist. This work is focused on the preparation of conventional reversed-phase stationary phases, and of non-conventional stationary phases, following three main steps. First, we developed a robust and efficient grafting protocol under microwave irradiations, and we studied the effect of thermal pretreatment on the final stationary phases. Then, the modified particles were completely characterized through a various and complementary set of analytical techniques. For the polar embedded aromatic stationary phase, molecular modeling through density functional theory calculations helped understanding the chromatographic results. The final step corresponded to the evaluation of the chromatographic properties of the stationary phases. By selecting the suitable test depending on the surface chemistry and the properties to be evaluated, the stationary phases developed were compared with those commercially available. Multivariate data analyses were carried out to define groups of columns and situate them in relation to those available on the market. Finally, the stationary phases developed during this thesis represent a wide range of columns.
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Mélanie Mignot. Elaboration de phases stationnaires originales pour la Chromatographie Liquide Haute Performance : Synthèse, caractérisation, et évaluation des propriétés chromatographiques des colonnes.. Chimie analytique. Université de Rouen, France, 2016. Français. ⟨tel-01674550⟩

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