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A method for preparing chromatogram stationery phase of rhein linked silica gel

A chromatographic stationary phase, bonded silica technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of little research on chromatographic separation function, limited to chiral recognition ability, etc.

Inactive Publication Date: 2006-11-22
NANCHANG UNIV
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  • Summary
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Problems solved by technology

[0009] The above research shows that the unique structure of natural compounds makes them inherently potential as chromatographic ligands, and artificially synthesized ligands often fail to reach this level. The existing development is limited to chiral recognition ability, and the chromatographic separation function of natural compounds remains to be seen. systematic research and development
However, at present, there are few studies on the direct use of the natural chromatographic separation function of active ingredients in Chinese herbal medicines, and the in-depth development and utilization of Chinese herbal medicine resources is of great significance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Take YQG 5μm (320m 2 / g) 100 g of spherical activated silica gel is used as the substrate.

[0027] (1) Under a nitrogen atmosphere, the γ- Aminopropyltriethoxysilane was added to anhydrous toluene, the oil bath was heated rapidly to 110°C, stirred, and reacted under reflux for 8 hours, and nitrogen was continued until room temperature; filtered, the solid was washed with toluene and methanol, and the solid was washed at 80°C Vacuum drying to obtain an amino group-containing silica gel precursor;

[0028] (2) Calculate rhein and thionyl chloride consumption by the unit consumption of activated silica gel (g) in step (1), be 2.3 by rhein (mmoL), thionyl chloride (mL) be the ratio of 1.9, the chlorine Add thionyl chloride to rhein, react under reflux for 2 hours, and vacuum evaporate the remaining thionyl chloride to obtain rhein acid chloride;

[0029] (3) calculate the anhydrous toluene consumption of triethylamine by the unit consumption of activated silica gel (g) ...

Embodiment 2

[0033] Take Kromasil 5μm (340m 2 / g) 50 g of spherical activated silica gel is used as the substrate.

[0034] (1) Under a nitrogen atmosphere, the γ-amino Add propyltrimethoxysilane to anhydrous toluene, heat the oil bath to 120°C rapidly, stir, and react under reflux for 10 hours, and continue to blow nitrogen until room temperature; filter, wash the solid with toluene and methanol, and dry under vacuum at 80°C , to prepare an amino group-containing silica gel precursor;

[0035] (2) Calculate rhein and thionyl chloride consumption by the unit consumption of activated silica gel (g) in step (1), be 2.7 by rhein (mmoL), thionyl chloride (mL) be the ratio of 2.2, chlorine Add thionyl chloride to rhein, react under reflux for 2.5 hours, and vacuum evaporate the remaining thionyl chloride to obtain rhein acid chloride;

[0036] (3) calculate the anhydrous toluene consumption of triethylamine by the unit consumption of activated silica gel (g) in step (1), be 0.44 by triethyla...

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Abstract

The invention relates to a process of preparing chromatographic fixed phase using functional coupling agent by means of secondset reaction, which comprises three steps: (1) preparing gamma-amino propyl bonding silica gel prosoma; (2) adding excess chlorinated sulfoxide into emodic acid for ereaction under regurgitation condition for 2 hours, vacuum boiling left chlorinated sulfoxide and getting emodic acid chloride; (3) proceeding reaction under regurgitation and stirring condition with protective nitrogen for 10 hours with prosoma and emodic acid chloride, taking waterless toluene as disslovant and triethylamine as catalyst; extracting, washing, floating and fdrying solid and preparing emodic acid bonding silica gel fixed phase. The invention is chartacterized by simple process, low production cost, high concentration of bonded ligand on surface of said fixed phase, and hardness for bacteria growth because of antibiotic action of emodic acid. The emodic acid bonded silica gel fixed phase is suitable for high efficiency liquid chromatography, microcylinder liquid chromatography and electrochromatography analysis and separation. It can also suit to be used as relative enriched material.

Description

technical field [0001] The invention relates to a preparation method of a silica gel chromatography stationary phase, in particular to a preparation method of a silica gel chromatography stationary phase using natural products as ligands. Background technique [0002] Compared with classical liquid chromatography (LC), high-performance liquid chromatography (HPLC) not only has higher separation efficiency, but also has good selectivity. It has become one of the important separation and analysis methods in the fields of inorganic, organic, biochemical, environmental, food and pharmaceutical analysis. . The basic requirement of chromatographic analysis is to achieve the separation of the components of the mixture. The essence of the separation is based on the difference in the interaction between the analyzed solute and the mobile phase and stationary phase. Among them, the development of new high-efficiency stationary phases is the core of the chromatographic system and has ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/29
Inventor 李来生黄志兵许丽丽王上文刘超
Owner NANCHANG UNIV
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