A silica gel chromatography packing with ordered mesoporous core-shell structure and its preparation and application

Abstract

The invention relates to a novel core-shell structure silica gel chromatographic filler suitable for ultrafast separation and its preparation and application. The silica gel microsphere synthesized by the invention has a clear core-shell structure, the core is non-porous silica gel, and the shell layer has mesopores. The first step is to synthesize non-porous silica gel with different particle sizes by temperature control method. This non-porous silica gel has good monodispersity and narrow particle size distribution. Then, a variety of cationic surfactants and organic amines are selected in the ammonia solution. or long-chain alkanes as pore-enlarging assistants, and a mesoporous shell with an adjustable thickness is prepared on this non-porous silica gel, which is controlled within the range of 100-360nm. The third step is to optimize the pore expansion of the mesoporous shell, according to To separate samples, adjust the pore size to 9nm, 15nm, or larger, and finally derivatize the silica gel microspheres to prepare a chromatographic stationary phase for rapid separation. The column efficiency is more than 200,000, which can be Fast and efficient separation of peptide and whole protein samples.

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 JosephJ. Sphere superposition growth method Adham Ahmed, Walid Abdelmagid, Harald Ritchie, Peter Myers, Haifei Zhang, J. Chromatogr.A, 2012, 1270, 194–203, etc. The layer-by-layer growth method has a cumbersome synthesis process, a long synthesis cycle, and easily leads to t...

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Problems solved by technology

Using cationic surfactants as templates, it can be used in traditional Core-shell silica gel microspheres SukBonYoon, Jong-YunKim, JungHoKim, YongJoonPark, KukRoYoon, Seung-KyuPark and Jong-SungYu, J.Mater.Chem., 2007, 17, 1758–1761 were synthesized in the system, and engraved The etchant uses silica gel to dissolve and then deposit to prepare core-shell silica particles Hanjiang Dong and John D. Brennan, J. Mater. Chem., 2012, 22, 13197–13203. From the point of view, the particle size or pore size of such microspheres is often difficult to meet the needs of chromatographic separation

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