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Preparation and application of pyridine ionic liquid functionalized beta-cyclodextrin silica gel chromatographic stationary phase

A pyridinium ion, cyclodextrin technology, applied in material separation, other chemical processes, chemical instruments and methods, etc., can solve the problems of complex preparation method and cumbersome process of β-cyclodextrin silica gel chromatography stationary phase, and achieve a good market. Application prospect, simple preparation process, easy operation effect

Active Publication Date: 2020-11-06
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the current preparation methods for ionic liquid functionalized β-cyclodextrin silica gel chromatography stationary phase are complicated, and each step of the experiment needs to be separated and purified, and the process is cumbersome

Method used

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  • Preparation and application of pyridine ionic liquid functionalized beta-cyclodextrin silica gel chromatographic stationary phase
  • Preparation and application of pyridine ionic liquid functionalized beta-cyclodextrin silica gel chromatographic stationary phase
  • Preparation and application of pyridine ionic liquid functionalized beta-cyclodextrin silica gel chromatographic stationary phase

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045]Ultrasonically disperse 3.0 g of γ-isocyanate triethoxysilane coupling agent and 3.0 g of silica gel microspheres in 30.0 ml of anhydrous pyridine solvent, raise the temperature to 75 ° C under the protection of nitrogen or argon atmosphere, and react with mechanical stirring for 24 h, then cool to room temperature; then 2.1g of β-cyclodextrin was added to the above reaction system, and the reaction was stirred at 70°C for 36 h; the β-cyclodextrin modified silica gel was obtained; after the mixture was cooled to room temperature, 2.1g of 3-bromopropane The base isocyanate was added dropwise to the above reaction suspension, stirred mechanically at 80°C for 72 h, cooled to room temperature, washed by centrifugation, and dried in vacuum to obtain the pyridine ionic liquid functionalized β-cyclodextrin silica gel chromatography stationary phase. The structure of the silica gel chromatography stationary phase is:

[0046]

[0047] The elemental analysis results show that ...

Embodiment 2

[0049] First, ultrasonically disperse 2.4 g of γ-isocyanate triethoxysilane coupling agent and 3.0 g of silica gel microspheres in 24.0 ml of anhydrous pyridine solvent, heat up to 80 °C under the protection of nitrogen or argon atmosphere, and react with mechanical stirring for 24 h , cooled to room temperature; then 2.1g of β-cyclodextrin was added to the above reaction system and stirred at 65°C for 36 h to obtain β-cyclodextrin-modified silica gel; after the mixture was cooled to room temperature, 1.5g of 2- Chloroethyl isocyanate was added dropwise to the above reaction suspension, stirred mechanically at 100°C for 24 hours, cooled to room temperature, washed by centrifugation, and dried in vacuum to obtain a pyridine ionic liquid functionalized β-cyclodextrin silica gel chromatography stationary phase. The structure of the silica gel chromatography stationary phase is:

[0050]

[0051] The elemental analysis results show that the bonding amount of each element of the...

Embodiment 3

[0053] First, ultrasonically disperse 3.6 g of γ-isocyanate trimethoxysilane coupling agent and 3.0 g of silica gel microspheres in 36.0 ml of anhydrous pyridine solvent, heat up to 50 °C under the protection of nitrogen or argon atmosphere and react mechanically for 48 h. Cool to room temperature; then add 3.0 g of β-cyclodextrin to the above reaction system and stir at 70 °C for 72 h to obtain β-cyclodextrin-modified silica gel; after the mixture is cooled to room temperature, continue to add 3.0 g of 2-bromoethyl Add the base isocyanate dropwise to the above reaction suspension and react with mechanical stirring at 70°C for 48h, then cool to room temperature, wash by centrifugation, and dry in vacuum to obtain the pyridine ionic liquid functionalized β-cyclodextrin silica gel chromatography stationary phase. The structure of the silica gel chromatography stationary phase is:

[0054]

[0055] Elemental analysis results show that the bonding amount of each element of the ...

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Abstract

The invention discloses a pyridine ionic liquid functionalized beta-cyclodextrin silica gel, which is prepared by the following steps of: ultrasonically dispersing silica gel microspheres and isocyanate silane into anhydrous pyridine, performing heating to 50-80DEG C under the protection of nitrogen or argon atmosphere, and carrying out stirring reaction for 24-48h; and adding beta-cyclodextrin into the reaction system, carrying out stirring reaction for 24-72h at a temperature of 60-80DEG C, adding halogenated isocyanate into the reaction system drop by drop, carrying out mechanical stirringreaction for 24-72h at a temperature of 60-100DEG C, carrying out centrifugal washing, and carrying out vacuum drying. Chromatographic separation selectivity results show that the pyridine ionic liquid functionalized beta-cyclodextrin silica gel prepared by the method has good chiral separation selectivity as compared with binaphthol chiral substances, benzoin chiral substances and alcohol chiralsubstances when used as a stationary phase.

Description

technical field [0001] The invention relates to the preparation and application of a liquid chromatography stationary phase, in particular to the preparation and application of a pyridine ionic liquid functionalized β-cyclodextrin silica gel chromatography stationary phase, which belongs to the technical field of novel chromatography stationary phases. Background technique [0002] Since the "seal baby" incident in Europe in the 1950s, people's requirements for the separation and analysis of chiral drugs have gradually increased, and the separation and analysis of enantiomers of active ingredients in drugs plays a vital role in drug development. High performance liquid chromatography (HPLC), as one of the important methods for the separation and analysis of enantiomers of synthetic drugs and natural products, mainly relies on the innovation of chiral chromatography stationary phase, so the development of new chiral chromatography Packing is the core of promoting the applicat...

Claims

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Application Information

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IPC IPC(8): B01J20/29B01J20/285G01N30/02
CPCG01N30/482B01J20/29B01J20/285G01N30/02Y02P20/54
Inventor 邱洪灯周行陈佳
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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