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Preparation method of organic-inorganic hybrid cyclodextrin chiral stationary phase

A chiral stationary phase and cyclodextrin technology, which is applied in chemical instruments and methods, and other chemical processes, can solve problems such as limiting the amount of cyclodextrin bonds, complex processes, and harsh reaction conditions, and achieve enhanced chiral separation performance, improving column permeability, and accelerating mass transfer

Inactive Publication Date: 2015-06-10
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the Chinese patent (CN 200410013253.9), Dashilu et al. used cyclodextrin sodium salt and bonded halopropyl group on the surface of silica gel to undergo solid phase condensation reaction to obtain cyclodextrin bonded silica gel stationary phase, but the process of this method is complicated , the reaction conditions are harsh, and the number of hydroxyl groups on the surface of silanol limits the amount of cyclodextrin bonding

Method used

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Examples

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Embodiment 1

[0023] Example 1 The preparation method of organic-inorganic hybrid cyclodextrin chiral stationary phase, the specific implementation steps are as follows:

[0024] (1) Preparation process of silicon-β-cyclodextrin derivatives

[0025] Put 3g of chlorotriazine-β-cyclodextrin, 2g of aminopropyltriethoxysilane and 1.5g of sodium bicarbonate in a round bottom flask filled with 50mL of water, and magnetically stir in a water bath at 50°C for 30min. After the reaction was completed, 80 mL of ethanol was added, and the silicon-β-cyclodextrin derivative precipitated out, and the precipitate was collected by filtration and dried for later use.

[0026] (2) Preparation of organic-inorganic hybrid cyclodextrin chiral stationary phase by hydrothermal synthesis

[0027] 0.3 g of silyl-β-cyclodextrin derivative prepared in step 1), 1.5 g of silylating agent 1,2-bis(trimethoxysilyl)ethane and 1 g of cetyltrimethylammonium bromide The surfactant was dissolved in 25mL of water, 12mL of etha...

Embodiment 2

[0031] Example 2 The preparation method of organic-inorganic hybrid cyclodextrin chiral stationary phase, the specific implementation steps are as follows:

[0032](1) Preparation process of silicon-β-cyclodextrin derivatives

[0033] Put 4g of chlorotriazine-β-cyclodextrin, 3g of aminopropyltriethoxysilane and 1.5g of sodium bicarbonate into a round bottom flask filled with 50mL of water, and magnetically stir in a water bath at 50°C for 30min. After the reaction was completed, 80 mL of ethanol was added, and the silicon-β-cyclodextrin derivative precipitated out, and the precipitate was collected by filtration and dried for later use.

[0034] (2) Preparation of organic-inorganic hybrid cyclodextrin chiral stationary phase by hydrothermal synthesis

[0035] 0.4 g of the silyl-β-cyclodextrin derivative prepared in step 1), 1.7 g of the silylating agent 1,2-bis(trimethoxysilyl)ethane and 1.2 g of hexadecyltrimethylchloride Ammonium surfactant was dissolved in 25mL of water, ...

Embodiment 3

[0039] Example 3 The preparation method of organic-inorganic hybrid cyclodextrin chiral stationary phase, the specific implementation steps are as follows:

[0040] (1) Preparation process of silicon-β-cyclodextrin derivatives

[0041] Put 5g of chlorotriazine-β-cyclodextrin, 4g of aminopropyltriethoxysilane and 1.5g of sodium bicarbonate into a round bottom flask filled with 50mL of water, and magnetically stir in a water bath at 50°C for 30min. After the reaction was completed, 80 mL of ethanol was added, and the silicon-β-cyclodextrin derivative precipitated out, and the precipitate was collected by filtration and dried for later use.

[0042] (2) Preparation of organic-inorganic hybrid cyclodextrin chiral stationary phase by hydrothermal synthesis

[0043] 0.4 g of the silyl-β-cyclodextrin derivative prepared in step 1), 1.7 g of the silylating agent 1,2-bis(trimethoxysilyl)ethane and 1.2 g of octadecyltrimethylchloride Ammonium surfactant was dissolved in 25mL of water,...

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Abstract

The invention discloses a preparation method of an organic-inorganic hybrid cyclodextrin chiral stationary phase. According to the method, a surfactant is taken as a template, a silicon-based-beta-cyclodextrin derivative and a silanization reagent are subjected to a hydro-thermal synthesis method to obtain the spherical organic-inorganic hybrid cyclodextrin chiral stationary phase, average aperture of silicon ball is 2.5 nanometers, and particle size is 5-8 micrometers. The preparation method has the advantages of mild reaction condition, simple preparation process and adjustable load capacity of the cyclodextrin derivative. The organic-inorganic hybrid cyclodextrin chiral mesoporous silicon ball stationary phase is not restricted by usage of a mobile phase polar solvent during a usage process, resolution efficiency is high, and chiral resolution capability is good.

Description

technical field [0001] The invention relates to a method for preparing an organic-inorganic hybrid cyclodextrin chiral mesoporous stationary phase. Specifically, silicon-based-β-cyclodextrin derivatives and silylating reagents are used as mixed silicon sources, and surfactants are used as templates. Hydrothermal synthesis methods are used to prepare cyclodextrin derivative groups in the channels. The spherical organic-inorganic hybrid cyclodextrin chiral mesoporous silicon sphere stationary phase with a pore diameter of 2.5 nanometers and a particle diameter of 5-8 microns. It is applied in the field of chiral separation of enantiomers by high performance liquid chromatography. Background technique [0002] Chirality is a fundamental feature in nature and life processes. There are major differences in the pharmacological properties of chiral drugs. One enantiomer of some chiral molecular drugs has good medicinal effects, while the other enantiomer has no medicinal effect o...

Claims

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Application Information

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IPC IPC(8): B01J20/29B01J20/30
Inventor 赵亮王利涛董树清张志欣张霞张晓莉
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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