Ordered mesopore core-shell structure silica gel chromatographic packing material, preparation and application of ordered mesopore core-shell structure silica gel chromatographic packing material

Abstract

The invention relates to a novel core-shell structure silica gel chromatographic packing material suitable for super rapid separation, preparation and application of the core-shell structure silica gel chromatographic packing material. A silica gel microsphere synthesized from the novel core-shell structure silica gel chromatographic packing material has a clear core-shell structure, a core is pore-free silica gels, and mesopores exist on a shell layer. The preparation method comprises the steps of 1. synthesizing pore-free silica gels with different particle sizes by adopting a program temperature control manner, wherein the pore-free silica gels are good in monodispersity and narrower in particle size distribution; 2. selecting multiple cationic surface active agents from an ammonia water solution and selecting organic amine or long-chain alkane as a reaming additive, preparing a mesopore shell layer the thickness of which can be adjusted on the pore-free silica gels, controlling the thickness to be within a range of 100-360nm; and 3. performing chambering optimization on the pore diameter of the mesopore shell layer, respectively adjusting the pore diameter to be 9nm, 15nm or more according to the requirement of separating samples, and finally, performing derivatization on the silica gel microsphere to prepare a chromatographic stationary phase. The novel core-shell structure silica gel chromatographic packing material is applied to rapid separation, with a column efficiency being above two hundred thousand, and polypeptide and integral protein samples can be rapidly and efficiently separated in a short time.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a process for preparing silica gel chromatography filler with mesoporous core-shell structure. technical background [0002] Fast and efficient is the development direction of chromatographic separation. Core-shell silica gel chromatography packing has the advantages of narrow particle size distribution and fast mass transfer speed, so it has become the first choice packing for fast chromatographic separation in recent years. At present, the preparation methods of core-shell structure chromatographic fillers that have been applied in chromatography include layer-by-layer growth method Joseph J.Kirkland, Timothy J.Langlois, US Patent, 2007 / 0189944A1, condensation method Wu Chen, Ta-Chen Wei, US Patent , 2011 / 0031179A1 and silicon sphere superposition growth method Adham Ahmed, Walid Abdelmagid, Harald Ritchie, Peter Myers, Haifei Zhang, J.Chromatogr.A, 201...

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Problems solved by technology

Using cationic surfactants as templates, it can be used in traditional Core-shell silica gel microspheres were synthesized in the system Suk Bon Yoon, Jong-Yun Kim, Jung Ho Kim, Yong Joon Park, Kuk Ro Yoon, Seung-Kyu Park and Jong-Sung Yu, J.Mater.Chem.,2007,17 ,1758–1761, it is also possible to add an etchant to this system and use silica gel to dissolve and then deposit to prepare core-shell structured silica gel particles Hanjiang Dong and John D.Brennan, J.Mater.Chem.,2012,22,13197– 13203, its pore structure can be perpendicular to the surface of silica spheres, but from the perspective of chromatographic separation, the particle size or pore size of such microspheres is often difficult to meet the needs of chromatographic separation

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