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Production method of chiral chromatographic column

A technology of a chiral chromatographic column and a production method, which is applied in the production field of the chiral chromatographic column and can solve the problems of the small application range of the chiral chromatographic column and the like

Inactive Publication Date: 2015-09-09
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The chiral chromatographic column prepared by chemical bonding, the separation effect depends entirely on the bonded chemical groups, and the scope of application of the chiral chromatographic column is small

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Add 5.2g tetraethoxysilane (TEOS) and 200ml ethanol solution to the beaker, mix well, add 3ml 0.375g / ml tetrabutylammonium hydroxide and amino acid derivatives mixed solution, stir at room temperature for 30min, then add 4ml Ammonia (NH 4 OH29.08%), the beaker was sealed with parafilm, and the colloidal suspension was stirred overnight at room temperature for reaction; after the reaction, the mixture was centrifuged at 3000r / min for 10min to separate the reaction product, and the reaction product was rinsed with ethanol solution (first-order washing), and then Place in a vacuum oven for vacuum drying. Take 3 g of the above dried sample and dissolve it in 200 ml of deionized water, stir for 2 hours, filter with suction and wash with deionized water (secondary washing). This process is repeated 4 to 5 times to obtain the mesoporous microsphere material.

[0015] The prepared mesoporous microsphere material was used as a stationary phase under a pressure of 5000 psi, homo...

Embodiment 2

[0017] Add 5.0g tetraethoxysilane (TEOS) and 200ml ethanol solution to the beaker, mix evenly, add 3ml of 0.375g / ml tetrabutylammonium hydroxide and amino acid derivative mixed solution, stir at room temperature for 30min, then add 4ml Ammonia (NH 4 OH 29.08%), the beaker was sealed with a parafilm, and the colloidal suspension was stirred and reacted at room temperature for 10h; after the reaction, the mixture was centrifuged at 3000r / min for 10min to separate the reaction product, and the reaction product was rinsed with ethanol solution (first-order washing), and then placed Carry out vacuum drying treatment in vacuum oven. Take 3 g of the above dried sample and dissolve it in 200 ml of deionized water, stir for 2 hours, filter with suction and wash with deionized water (secondary washing). This process is repeated 4 to 5 times to obtain the mesoporous microsphere material.

[0018] The prepared mesoporous microsphere material was used as a stationary phase under a pressur...

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Abstract

The invention relates to a production method of a chiral chromatographic column. The production method comprises the following steps: stirring and mixing a silicon source, an ethanol solution, a template solution and ammonia water for hybrid reaction at an indoor temperature; after the reaction is finished, recycling a reaction product and performing impurity removal treatment so as to obtain a mesoporous microsphere material; an empty column is filled with the mesoporous microsphere material made by use of a homogenation method, and a homogenate is prepared by mixing THF (Tetra Hydro Furan) and N-methyl pyrrolidone. According to the production method of chiral chromatographic column, the mesoporous microsphere material is prepared by taking tetrabutyl ammonium hydroxide and amino acid derivatives as templates, and tetraethoxysilane as a silicon source, and the empty column is filled with the mesoporous microsphere material by use of the homogenation method so as to obtain the chiral chromatographic column; HPLC (High Performance Liquid Chromatography) chiral separation is performed on an enantiomer by use of a special channel formed by use of the templates (etrabutyl ammonium hydroxide and the amino acid derivatives), the applicable scope of the selective separation is wide, and the chiral chromatographic column is applicable to separation of different enantiomers.

Description

technical field [0001] The invention relates to the field of chromatographic column production, in particular to a production method of a chiral chromatographic column. Background technique [0002] By introducing a chiral environment, the chiral chromatographic column makes the adsorption of enantiomers to the chiral column show differences, so as to achieve the purpose of optical isomer resolution. Most of the existing chiral chromatographic columns are produced by bonding chemical groups on the surface of the chromatographic column packing. The separation effect of the chiral chromatographic column prepared by chemical bonding depends entirely on the bonded chemical groups, and the scope of application of the chiral chromatographic column is small. Contents of the invention [0003] The object of the present invention is to provide a production method of a chiral chromatographic column, which can effectively solve the above problems, and the prepared chiral chromatogra...

Claims

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Application Information

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IPC IPC(8): B01D15/38B01J20/10B01J20/28B01J20/30
Inventor 顾昊李秀珍
Owner BEIJING INSTITUTE OF TECHNOLOGYGY