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Cyclodextrin linkage silica gel fixed phase, preparing method and use thereof

A technology of bonding silica gel and cyclodextrin, which is applied to chemical instruments and methods, other chemical processes, instruments, etc., can solve the problems of separation selectivity, cumbersome operation, easy hydrolysis, etc., to improve the symmetry of chromatographic peaks, reduce Separation and purification, increase the effect of reactivity

Inactive Publication Date: 2005-02-23
WUHAN UNIV
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Problems solved by technology

But then it was found that the nitrogen-containing spacer cyclodextrin bonded stationary phase has the following disadvantages: (1) unstable and easy to hydrolyze; (2) separation selectivity is affected by the spacer; (3) during the synthesis process, nitrogen Unavoidable partial oxidation makes the stationary phase yellow; (4) The synthesis process is long and cumbersome to operate
Our laboratory used this spacer to prepare natural and derivatized cyclodextrin bonded stationary phases, but the separation selectivity was poor and there was no chiral resolution performance.
Armstrong et al. also prepared a cyclodextrin bonded stationary phase through a series of coupling agents containing epoxy functional groups, and their natural cyclodextrin bonded silica gel immobilized enantiomeric separation selectivity is not good.

Method used

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  • Cyclodextrin linkage silica gel fixed phase, preparing method and use thereof
  • Cyclodextrin linkage silica gel fixed phase, preparing method and use thereof
  • Cyclodextrin linkage silica gel fixed phase, preparing method and use thereof

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preparation example Construction

[0015] 1. Preparation of cyclodextrin-bonded silica gel stationary phase

[0016] 1.1 Preparation of halopropyl-bonded silica gel

[0017] According to the ratio of silica gel: coupling agent: anhydrous toluene: 1g: 5mmoL: 50ml, add 150ml freshly distilled anhydrous toluene (anhydrous toluene is prepared by refluxing metal sodium to remove water) into a 250ml three-necked flask, and quickly add activated particle silica gel (particle size 5 μm, Kromasil, Sweden), and then add halopropyltriethoxysilane coupling agent. Protected by dry nitrogen (the nitrogen has been pre-dried by concentrated sulfuric acid and calcium chloride), under magnetic stirring, add 3 drops (about 0.1ml) of freshly distilled triethylamine dropwise, and the oil bath is heated rapidly to 110-120°C, and react under reflux After 24 hours (a drying tube with anhydrous calcium chloride is installed on the upper end of the condensation tube), suction filter with a G-4 sand core funnel while it is hot, and wash...

specific Embodiment approach

[0018] 1. Preparation of cyclodextrin-bonded silica gel stationary phase

[0019] 1.1 Preparation of activated silica gel

[0020] Suspend silica gel (particle size 5 μm, Kromasil, Sweden) in 6 mol / L hydrochloric acid, the mass ratio of silica gel to hydrochloric acid volume is 1 g: 15-20 ml. Reflux for 24 hours under stirring, filter with a G-4 sand core funnel while it is hot, wash the solid repeatedly with water twice to neutrality, and wash it with acetone three times, dry it under an infrared lamp until the silica gel is dispersed, and then dry it in an oven at 160°C After more than 10 hours, take it out and place it in a desiccator to cool to room temperature, quickly transfer it to a vacuum drying gun, heat it in a water bath, and dry it in vacuum for more than 16 hours to obtain activated silica gel.

[0021] 1.2 Preparation of halopropyl-bonded silica gel

[0022] According to the ratio of silica gel: coupling agent: anhydrous toluene: 1g: 5mmoL: 50ml, add 150ml fre...

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Abstract

A cyclodextrin bonded silica gel and fixing phase for efficient liquid-phase chromatography is prepared through preparing and purifying the halopropyl bonded silica gel, reacting between sodium hydride and cyclodextrin to obtain cyclodextrin sodium, and solid-phase condensing reacting between said cyclodextrin sodium and halopropyl bonded silica gel.

Description

technical field [0001] The invention relates to a cyclodextrin-bonded silica gel chromatographic stationary phase and its preparation method and application, which belongs to the synthesis technology of functional materials in methodology; its object belongs to a separation medium, and is suitable for high-performance liquid chromatography, micro-column liquid chromatography and electrochromatography, etc. Separation of scientific and technical fields. Background technique [0002] High-performance liquid chromatography plays a pivotal role in modern separation and analysis, and is widely used in chemistry, biology, medicine, life science and environmental science, and has become an indispensable research method. The separation system is becoming more and more complex, especially the separation and analysis of actual samples puts forward higher requirements for chromatographic technology, especially chromatographic stationary phase. At present, there are many types of commer...

Claims

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Application Information

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IPC IPC(8): B01J20/22
Inventor 达世禄冯钰锜刘敏李来生
Owner WUHAN UNIV
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