Versatile ene-thiol photoclick reaction for preparation of multimodal monolithic silica capillary columns

Abstract : This paper presents a photografting process of monolithic silica capillary columns based on the ene-thiol click chemistry. This study is performed on a "generic" vinyl-functionalized silica monolith (Hmin 6 ± 1 μm). The photoclick reaction is investigated using different thiol monomers (octadecanethiol, cysteine and sodium mercaptoethanesulfonate) to prepare capillary columns dedicated to various chromatographic modes (reversed-phase, HILIC and strong cation exchange). Whatever the monomer used, the photografting reaction is achieved in less than 5 min with a relatively high thiol monomer content. This allows preparing highly retentive and efficient monolithic columns while avoiding polymerization and/or column clogging. In addition to the aforementioned properties (duration, versatility, efficiency), this photo-triggered chemical reaction allows addressing several appropriate surface functionalizations inside a single monolithic column in order to prepare nanovolume multimodal capillary columns. A multimodal biphasic monolithic column with a 1 cm length cation-exchange segment followed by a 9 cm length reversed-phase segment (SCX-RP) is prepared through two successive photografting reactions using a UV-mask to localize the reactions. This multimodal biphasic column is investigated using a model sample for the selective fractionation and separation of cationic and neutral compounds and is applied to the on-line preconcentration and separation of β-blockers.
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Submitted on : Friday, October 10, 2014 - 2:23:57 PM
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Audrey Maréchal, A. Laaniste, Racha El Debs, Vincent Dugas, Claire Demesmay. Versatile ene-thiol photoclick reaction for preparation of multimodal monolithic silica capillary columns. Journal of Chromatography A, Elsevier, 2014, 1365, pp.140-147. ⟨10.1016/j.chroma.2014.09.017⟩. ⟨hal-01073802⟩



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