title: 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±1μm). 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 5min 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 1cm length cation-exchange segment followed by a 9cm 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.
authors.affiliation: Université de Lyon, Université Claude Bernard Lyon I, Institut des Sciences Analytiques, UMR CNRS 5280, 5, rue de la DOUA, 69100 Villeurbanne, France.
authors.forename: A
authors.initials: A
authors.lastname: Marechal
authors.affiliation: Université de Lyon, Université Claude Bernard Lyon I, Institut des Sciences Analytiques, UMR CNRS 5280, 5, rue de la DOUA, 69100 Villeurbanne, France.
authors.forename: A
authors.initials: A
authors.lastname: Laaniste
authors.affiliation: Université de Lyon, Université Claude Bernard Lyon I, Institut des Sciences Analytiques, UMR CNRS 5280, 5, rue de la DOUA, 69100 Villeurbanne, France.
authors.forename: R
authors.initials: R
authors.lastname: El-Debs
authors.affiliation: Université de Lyon, Université Claude Bernard Lyon I, Institut des Sciences Analytiques, UMR CNRS 5280, 5, rue de la DOUA, 69100 Villeurbanne, France. Electronic address: vincent.dugas@univ-lyon1.fr.
authors.forename: V
authors.initials: V
authors.lastname: Dugas
authors.affiliation: Université de Lyon, Université Claude Bernard Lyon I, Institut des Sciences Analytiques, UMR CNRS 5280, 5, rue de la DOUA, 69100 Villeurbanne, France.
authors.forename: C
authors.initials: C
authors.lastname: Demesmay
mesh_terms: D002852:Chromatography, Ion Exchange / Q000295:instrumentation; D056148:Chromatography, Reverse-Phase / Q000295:instrumentation; D057930:Click Chemistry; D007536:Isomerism; D055668:Photochemical Processes; D012822:Silicon Dioxide / Q000737:chemistry*; D013438:Sulfhydryl Compounds / Q000737:chemistry*
chemical_list: D013438:Sulfhydryl Compounds; D012822:Silicon Dioxide
keywords: Biphasic capillary column; HILIC; Multimodal chromatography; Photografting; SCX; Silica monolithic columns