Temperature response type beta-cyclodextrin silica gel stationary phase and preparation method thereof

A temperature-responsive, cyclodextrin technology, applied in the field of liquid chromatography stationary phase preparation, can solve the problems of limited types of temperature-sensitive chromatographic packing materials, and achieve the effects of avoiding non-specific adsorption, flexible application, and novel structure

Inactive Publication Date: 2014-09-10
NINGXIA UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Nevertheless, the types of temperature-sensitive chromatographic packing are still very limited, and its retention mechanism needs t...

Method used

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  • Temperature response type beta-cyclodextrin silica gel stationary phase and preparation method thereof
  • Temperature response type beta-cyclodextrin silica gel stationary phase and preparation method thereof
  • Temperature response type beta-cyclodextrin silica gel stationary phase and preparation method thereof

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Embodiment 1

[0027] Preparation of β-cyclodextrin derivatives

[0028] Dissolve 20.0g of sodium hydroxide in 800mL of distilled water, add 40.0g of β-cyclodextrin, under vigorous stirring at 0-5°C, add 40.0g of p-toluenesulfonyl chloride to react for 5 hours; filter, cool the filtrate to 0°C, wash with hydrochloric acid Adjust the pH to 6-7 and store in the refrigerator overnight to obtain a white solid product; wash and dry to obtain benzoylated β-cyclodextrin. ;

[0029] Weigh 10.0g of benzoylated β-cyclodextrin, then add 60mL of ethylenediamine, stir and react in a 75°C water bath for 4 hours; then add dropwise to the above reaction solution into 500mL of cold acetone, and immediately form a white precipitate , filter under reduced pressure, redissolve the white precipitate in 60mL water / methanol (v / v=3:1) mixed solution, filter to obtain a light yellow clear liquid; slowly pour the light yellow clear filtrate into 200mL acetone, reduce pressure Collect the white precipitate by filtra...

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Abstract

The invention relates to a temperature response type beta-cyclodextrin silica gel stationary phase. The structural formula of the temperature response type beta-cyclodextrin silica gel stationary phase is as shown in the specification. The preparation method comprises the steps of deriving beta-cyclodextrin to obtain a beta-cyclodextrin derivative with a reaction group and a functional group, then performing silylation reaction, modifying a silica gel surface with a silylation reagent with two bonds, performing polymerization reaction on acrylamide and a glycidyl ether monomer to form a meshed temperature-sensitive polymer layer on the silica gel surface through azodiisobutyronitrile serving as an initiator, and finally implanting the beta-cyclodextrin derivative into a polymer chain to obtain the temperature response type beta-cyclodextrin silica gel stationary phase. The preparation process is simple, and the property is stable; the prepared temperature response type beta-cyclodextrin silica gel stationary phase can overcome the shortcomings that silica gel cannot resist water and alkali and undergoes non-specific adsorption; a prepared separation material is novel in structure and flexible in application; effective separation of compounds can be realized by controlling the column temperature; furthermore, the beta-cyclodextrin derivative in the polymer chain can improve the hydrophilicity and the chiral recognition capacity of the stationary phase, and is suitable for separation and chiral separation of polar and hydrophilic compounds and chemical molecules.

Description

technical field [0001] The invention relates to a method for preparing a liquid chromatography stationary phase, in particular, provides a method for preparing a high performance liquid chromatography temperature-responsive silica gel stationary phase. Background technique [0002] Water-soluble, temperature-sensitive polymers are very attractive functional polymer materials in recent years. Since it was discovered in the late 1970s that lightly ionized polyacrylamide has a volume phase transition phenomenon in a specific medium, people have studied a series of factors that cause its volume phase transition, such as temperature, pressure, solvent composition, and pH value. and ionic strength have been studied in depth. In recent years, this kind of temperature-sensitive polymer gel has shown broad application prospects in the fields of controlled release of drugs, separation of substances, and immobilized enzymes. There are continuous reports on the use of heat-sensitive...

Claims

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Application Information

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IPC IPC(8): B01J20/29B01J20/30C08F292/00C08F8/32C08B37/16
Inventor 李媛媛刘莉
Owner NINGXIA UNIVERSITY
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