Preparation method of capillary electro-chromatography column taking beta-cyclodextrin as bonded stationary phase and application in chiral drug separation

A technology of capillary electrochromatography and cyclodextrin, which is applied in the separation of chiral drugs, and in the field of preparation of capillary electrochromatographic columns, can solve the problems of separation of chiral drugs, and achieve low price, easy preparation, and low environmental pollution. Effect

Inactive Publication Date: 2013-02-13
ZHENGZHOU UNIV
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Problems solved by technology

[0006] In view of the above situation, in order to solve the defects of the prior art, the purpose of the present invention is to provide a preparation method of a capillary electrochromatographic column with β

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  • Preparation method of capillary electro-chromatography column taking beta-cyclodextrin as bonded stationary phase and application in chiral drug separation
  • Preparation method of capillary electro-chromatography column taking beta-cyclodextrin as bonded stationary phase and application in chiral drug separation

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preparation example Construction

[0030] ③. Preparation of silanized silica gel:

[0031] The present invention uses γ-(2,3-epoxypropoxy)propyltrimethoxysilane (KH-560) as a support, and the ethoxy group of KH-560 reacts with the silicon hydroxyl group on the surface of silica gel to prepare silanized silica gel. Namely silica gel KH-560.

[0032] The present invention bonds KH-560 to the surface of silica gel through -Si-O-Si- bonds. Due to the steric hindrance effect, it is impossible for the three methoxy groups of KH-560 to react with silanol groups, and the methoxy groups can be hydrolyzed into hydroxyl groups under aqueous conditions. Therefore, this reaction must be carried out under anhydrous conditions.

[0033] a Handling of reagents and utensils

[0034] Molecular sieves (molecular sieves are crystalline silicates or aluminosilicates, which are formed by connecting silicon-oxygen tetrahedrons or aluminum-oxygen tetrahedrons through oxygen bridges, and are usually pore and cavity systems with a mo...

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Abstract

The invention relates to a preparation method of a capillary electro-chromatography column taking beta-cyclodextrin as a bonded stationary phase and an application in a chiral drug separation, and can effectively solve the problems of the capillary electro-chromatography column preparation and the chiral drug separation. The solved technical proposal comprises the following steps: (1) preparing six-bit mono substituted P-toluenesulfonyl-beta-cyclodextrin, (2) preparing six-bit mono substituted ammoniated-beta-cyclodextrin, (3) preparing silylated silica gel, (4) preparing a beta-cyclodextrin bonded silica gel chiral stationary phase, and (5) preparing a capillary packing column. The preparation method is low in cost, low in toxicity and low in environment pollution, and is an innovation of the preparation method of the capillary electro-chromatography column taking the beta-cyclodextrin as the bonded stationary phase and the application in the chiral drug separation.

Description

technical field [0001] The invention relates to a separation technology, in particular to a preparation method of a capillary electrochromatographic column using β-cyclodextrin as a bonded stationary phase and its application in separation of chiral drugs. Background technique [0002] Capillary electrochromatography is currently a relatively new separation technique, which is mainly based on the chromatographic separation mechanism. Fill, coat or bond the stationary phase in the capillary so that the separated components are retained and distributed in the stationary phase. Since capillary electrochromatography is a separation technique based on the combination of liquid chromatography and capillary electrophoresis, it has good selectivity and high separation efficiency. According to different packing methods of stationary phase, capillary electrochromatography can be divided into three subtypes, namely open-tubular capillary column (OTC-CEC), packed capillary column (PC-C...

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Application Information

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IPC IPC(8): B01D15/22B01J20/26C07B57/00C07C209/88C07C211/42C07C213/10C07C215/68C08G83/00C08B37/16
Inventor 周婕张振中刘倩郑旭霞叶凡
Owner ZHENGZHOU UNIV
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