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Cation exchange chromatography stationary phase and preparation method thereof

A chromatographic stationary phase and cation exchange technology, applied in the field of new liquid chromatography stationary phase and its preparation, can solve the problem of less silica matrix, and achieve the effects of good separation selectivity, novel structure and industrialization.

Inactive Publication Date: 2015-01-14
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to problems such as the surface modification method of silica gel and the chemical stability of silica gel, silica gel matrix is ​​less used in ion exchange chromatography.
However, there are currently no techniques for preparing stationary phases for ion-exchange chromatography using this method

Method used

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  • Cation exchange chromatography stationary phase and preparation method thereof
  • Cation exchange chromatography stationary phase and preparation method thereof
  • Cation exchange chromatography stationary phase and preparation method thereof

Examples

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Effect test

Embodiment 1

[0025] Weigh 10g spherical silica gel (particle size is 5μm, pore size is 10nm, specific surface area is 305m 2 / g), placed in a 250mL glass flask, added 150mL of 10% hydrochloric acid solution, heated to reflux for 12 hours, cooled to room temperature, filtered, washed with water until neutral, and dried at 150°C for 24 hours. Under the condition of blowing dry nitrogen, 80 mL of dry toluene was added to the hydrated silica gel, stirred evenly, and then 6 mL of diethylphosphorylethyltriethoxysilane was added dropwise, and the reaction was stirred at 50°C for 24 hours. The reaction system was filtered, washed successively with toluene, dichloromethane, methanol, water, tetrahydrofuran, and methanol, and the product was dried at 60°C for 12 hours. Take 10g of the above-mentioned bonded silica gel, put it in a 250mL glass flask, add 100ml of 10% hydrochloric acid aqueous solution, stir at 50°C for 12 hours, cool the reaction system to room temperature, filter under reduced press...

Embodiment 2

[0027] Weigh 10g spherical silica gel (particle size is 5μm, pore size is 10nm, specific surface area is 305m 2 / g), placed in a 250mL glass flask, added 150mL of sulfuric acid solution with a volume concentration of 10%, heated to reflux for 12 hours, cooled to room temperature, filtered, washed with water until neutral, and dried at 150°C for 24 hours. Under the condition of blowing dry nitrogen, 80 mL of dry toluene was added to the silica gel, stirred evenly, then 6 mL of diethylphosphorylethyltriethoxysilane was added dropwise, and the reaction was stirred at 50°C for 24 hours. The reaction system was filtered, washed successively with toluene, dichloromethane, methanol, water, tetrahydrofuran, and methanol, and the product was dried at 60°C for 12 hours. Take 10g of the above-mentioned bonded silica gel, put it in a 250mL glass flask, add 100ml of 10% sulfuric acid aqueous solution, stir at 50°C for 12 hours, cool the reaction system to room temperature, filter under red...

Embodiment 3

[0029] Weigh 10g spherical silica gel (particle size is 5μm, pore size is 10nm, specific surface area is 305m 2 / g), placed in a 250mL glass flask, added 150mL of 10% hydrochloric acid solution, heated to reflux for 12 hours, cooled to room temperature, filtered, washed with water until neutral, and dried at 150°C for 24 hours. Under the condition of blowing dry nitrogen, 80 mL of dry toluene was added to the silica gel, stirred evenly, and then 6 mL of diethylphosphorylethyltriethoxysilane was added dropwise, and the reaction was stirred at 70°C for 24 hours. The reaction system was filtered, washed successively with toluene, dichloromethane, methanol, water, tetrahydrofuran, and methanol, and the product was dried at 60°C for 12 hours. Take 10g of the above-mentioned bonded silica gel, put it in a 250mL glass flask, add 100ml of 70% hydrochloric acid aqueous solution, stir at 50°C for 12 hours, cool the reaction system to room temperature, filter under reduced pressure and w...

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Abstract

The invention relates to a liquid chromatography stationary phase, which is characterized in that a ligand is an alkyl and phosphate bonded phase, and the structural formula is as shown in the specification, wherein Silica Gel is silica gel and M = 0-16. The invention also provides a preparation method of the liquid chromatography stationary phase, and alkyl silane and phosphate silane are bonded to silica gel surface by silica gel surface bonding method. The liquid chromatography stationary phase is novel in structure, is provided with negative charges on the surface, and the surface charge density can be controlled, and the liquid chromatography stationary phase is very suitable for using as a strong cation exchange chromatography stationary phase, and can be widely used for separation and analysis of all kinds of cationic compounds.

Description

technical field [0001] The invention relates to a novel liquid chromatography stationary phase and a preparation method thereof, in particular to a novel cation exchange chromatography stationary phase whose ligands are alkyl groups and phosphoric acid groups. Background technique [0002] Ion exchange chromatography is widely used in the separation, analysis and purification of ionic substances (covering various types of substances from biological macromolecules to small inorganic ions). The research and development of ion exchange chromatography separation media is the basis for the development and application of ion exchange chromatography. Organic polymer separation media such as resins are widely used in ion exchange chromatography, and have the advantages of wide pH range and good stability [Nair, L.M. et al, J. Chromatogr. A, 1996, 739, 99]. However, organic polymer ion-exchange stationary phases have disadvantages such as poor mechanical strength, low separation eff...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01J20/30
CPCB01J20/286B01J2220/54B01J2220/80
Inventor 梁鑫淼郭志谋董雪芳
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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