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...

Examples

Embodiment

[0030] Non-porous silica gel synthesis

[0031] First prepare the hydrolyzate, 6.70ml of ammonia water (28-30wt.%, Sigma-Aldrich), 5.13ml of water, 69.55ml of absolute ethanol, stir mechanically in a water bath at 22°C; quickly add 4ml of ethyl orthosilicate to the hydrolyzate Esters (98%, Sigma-Aldrich), start the reaction, after 40min, raise the temperature of the water bath to 55°C, add 0.64ml of water and 4ml of ethyl orthosilicate, the ethyl orthosilicate must be preheated at 55°C in advance, the reaction 40min. After adding 0.64ml of water and 4ml of ethyl orthosilicate repeatedly for 3 times, add the hydrolyzate again (6.7ml of ammonia water (28-30wt.%, Sigma-Aldrich), 5.13ml of water, 69.55ml of absolute ethanol), and continue to add 0.64 ml water and 4 ml tetraethyl orthosilicate to grow to target particle size. After growing 7 layers, the synthetic non-porous silica gel was centrifuged and washed at 3000 rpm for 5 min, washed three times with ethanol and twice with...

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...

Examples

Embodiment

[0030] Non-porous silica gel synthesis

[0031] First prepare the hydrolyzate, 6.70ml of ammonia water (28-30wt.%, Sigma-Aldrich), 5.13ml of water, 69.55ml of absolute ethanol, stir mechanically in a water bath at 22°C; quickly add 4ml of ethyl orthosilicate to the hydrolyzate Esters (98%, Sigma-Aldrich), start the reaction, after 40min, raise the temperature of the water bath to 55°C, add 0.64ml of water and 4ml of ethyl orthosilicate, the ethyl orthosilicate must be preheated at 55°C in advance, the reaction 40min. After adding 0.64ml of water and 4ml of ethyl orthosilicate repeatedly for 3 times, add the hydrolyzate again (6.7ml of ammonia water (28-30wt.%, Sigma-Aldrich), 5.13ml of water, 69.55ml of absolute ethanol), and continue to add 0.64 ml water and 4 ml tetraethyl orthosilicate to grow to target particle size. After growing 7 layers, the synthetic non-porous silica gel was centrifuged and washed at 3000 rpm for 5 min, washed three times with ethanol and twice with...

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