Preparation method of alkali-resistant silica gel chromatographic column filling material

A silica gel chromatography and alkali-resistant technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of low coverage density of organic layer on the surface of silica gel chromatography packing, collapse of silica packing matrix, reduction of resolution and column efficiency, etc. To achieve the effect of weak residual silanol effect, small molecular loss and small impact

Inactive Publication Date: 2012-06-13
UNIV OF JINAN
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  • Abstract
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AI Technical Summary

Problems solved by technology

First of all, the organic layer coverage density on the surface of the silica gel chromatography filler prepared by the two-step bonding method is low. Long-term use of buffer salt or alkaline solution mobile phase will cause the silica gel filler matrix to collapse, the stationary phase will be lost, and the chromatographic column will be scrapped.
Secondly, most of the silanol groups did not participate in the reaction due to low reactivity during the stationary phase bonding reaction, even if there was a steric hindrance effect of the stationary phase molecules on the silica gel surface during the capping reaction, resulting in residual silanol groups exceeding 50% of the total number of original silanol groups. %
On the one hand, the residual silanol makes the surface of the silica gel easy to be hydrophilic, which leads to a decrease in life under alkaline conditions; Tailing, reduced resolution and column efficiency

Method used

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  • Preparation method of alkali-resistant silica gel chromatographic column filling material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1: the preparation of alkali-resistant carbon-octave silica gel chromatographic packing

[0026] Include the following steps A and B in turn:

[0027] A. Preparation of surface organohybrid silica gel

[0028] Add 5.0 g of activated fully porous spherical silica gel into the reaction vessel, add 50 ml of toluene, stir evenly, add 0.5 g of ethylene bridged hexaethoxysilane, protect it with high-purity nitrogen, and stir and reflux for 12 hours. Cool after the reaction, filter with suction, wash with 200ml of toluene, 200ml of ethanol, 200ml of ethanol-water (v / v, 1:1), 200ml of water, 200ml of methanol in turn, and dry in vacuum at 70°C for 12h to obtain the surface ethylidene complex. Silicone.

[0029] B. Preparation of alkali-resistant silica gel chromatography packing

[0030] Add 5.0g surface ethylene hybrid silica gel into the reaction vessel, add 50ml toluene, stir evenly, add 2.5g octadecyldimethylchlorosilane, protect with high-purity nitrogen, sti...

Embodiment 2

[0031] Embodiment 2: Preparation of alkali-resistant C12 silica gel chromatographic packing

[0032] Include the following steps A and B in turn:

[0033] A. Preparation of surface organohybrid silica gel

[0034] Add 5.0 g of activated fully porous spherical silica gel into the reaction vessel, add 50 ml of toluene, stir evenly, add 0.25 g of methyltriethoxysilane, protect with argon, and stir and reflux for 12 hours. After the reaction is completed, cool, filter with suction, wash with 200ml of toluene, 200ml of ethanol, 200ml of ethanol-water (v / v, 1:1), 200ml of water, and 200ml of methanol, and dry in vacuum at 70°C for 12h to obtain a surface methyl hybrid. Silica gel.

[0035] B. Preparation of alkali-resistant silica gel chromatography packing

[0036] Add 5.0g of surface methyl hybrid silica gel into the reaction vessel, add 50ml of toluene, stir evenly, add 5.0g of dodecyltrimethoxysilane, protect with high-purity nitrogen, stir and reflux for 24h. After the reac...

Embodiment 3

[0037] Embodiment 3: the preparation of alkali-resistant carbon eight silica gel chromatographic packing

[0038] Include the following steps A and B in turn:

[0039] A. Preparation of surface organohybrid silica gel

[0040]Add 5.0 g of activated fully porous spherical silica gel into the reaction vessel, add 50 ml of toluene, stir evenly, add 0.125 g of ethyltrimethoxysilane, protect with high-purity nitrogen, and stir to reflux for 12 hours. After the reaction is completed, cool, filter with suction, wash with 200ml of toluene, 200ml of ethanol, 200ml of ethanol-water (v / v, 1:1), 200ml of water, and 200ml of methanol, and dry in vacuum at 70°C for 12h to obtain a surface ethyl hybrid. Silica gel.

[0041] B. Preparation of alkali-resistant silica gel chromatography packing

[0042] Add 5.0g surface ethyl hybrid silica gel into the reaction vessel, add 50ml toluene, stir evenly, add 3.0g octyldimethylmethoxysilane, protect with high-purity nitrogen, stir and reflux for 3...

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Abstract

The invention discloses a preparation method of an alkali-resistant silica gel chromatographic column filling material. The preparation method provided by the invention comprises the following steps of preparing a silica gel matrix of which the surface has alkali resistance by a short-carbon chain silane coupling agent-based silica gel surface organic hybridization method, and carrying out stationary phase bonding. The preparation method is characterized in that a part of silanol groups on a totally porous spherical silica gel surface undergo bonding reactions in the presence of a short-carbon chain silane coupling agent so that the totally porous spherical silica gel surface is covered partly with short carbon chains, and thus organic hybridization of the totally porous spherical silica gel surface is realized and alkali-resistant silica gel having a thin and uniform organic covering layer is obtained; and through surface stationary phase bonding and last end-capping, the alkali-resistant silica gel chromatographic column filling material is obtained. The alkali-resistant silica gel chromatographic column filling material obtained by the preparation method has good alkali resistance, reduces a residual silanol effect, covers metal impurities on a silica gel surface, and has good application potentials.

Description

technical field [0001] The invention belongs to a preparation method of high-performance liquid chromatography silica gel packing, and particularly relates to the preparation of an alkali-resistant silica gel matrix by adopting a silica gel surface organic hybridization technology, and then bonding a stationary phase to prepare an alkali-resistant silica gel chromatography packing. The prepared silica gel chromatographic filler has a long service life under alkaline mobile phase conditions, can also weaken the effect of residual silanol to facilitate the separation of basic compounds, and can cover metal impurities on the surface of silica gel to eliminate non-specific adsorption. Background technique [0002] Prolonging the service life of chromatographic fillers and reducing the effect of residual silanol have always been the research content of chromatographic workers. Traditional silica-based HPLC packings are usually prepared by a two-step bonding reaction, that is, the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30
Inventor 孙敏罗川南
Owner UNIV OF JINAN
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