Bonding type chromatographic column stationary phase and preparation method thereof

A chromatographic column and stationary phase technology, applied in the field of chromatographic separation, can solve the problems of unstable alkaline medium, complex modification process, small specific surface area, etc., achieve stability and good hydrolysis resistance, simple process route, high specific surface area, etc. The effect of surface area

Active Publication Date: 2016-01-13
上海熙华检测技术服务股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Silica gel matrix is ​​widely used in liquid chromatography due to its good mechanical strength, chemical resistance and thermal stability; however, the exis

Method used

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  • Bonding type chromatographic column stationary phase and preparation method thereof
  • Bonding type chromatographic column stationary phase and preparation method thereof
  • Bonding type chromatographic column stationary phase and preparation method thereof

Examples

Experimental program
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[0033] Example one

[0034] 1. Weigh 4g of silica gel balls with a particle size of 5mm and place them in an eggplant-shaped bottle, add 50mL of 4mol / L hydrochloric acid aqueous solution, and reflux for 2 hours at room temperature to obtain a mixture;

[0035] 2. Carry out suction filtration of the mixture obtained above, wash the filter cake obtained by suction filtration with a large amount of deionized water until the filtrate is neutral, then wash the solids with acetone and ether respectively, and finally place it in a vacuum drying oven at room temperature Dry overnight

[0036] 3. Disperse 450 mg of the solid obtained in step 2 ultrasonically in 25 mL of deionized water, and add 335 mg of surfactant cetyltrimethylammonium bromide, 135 mL of absolute ethanol, 200 mL of deionized water, 2.5 mL of a mixed solution of saturated ammonia;

[0037] 4. Under the stirring condition of 1500rpm, quickly add 225μL 4,4'-bis(triethoxysilyl)-1,1'-biphenyl to the mixed solution obtained in st...

Example Embodiment

[0041] Example two

[0042] 1. Weigh 4g of silica gel balls with a particle size of 5mm and place them in an eggplant-shaped bottle, add 50mL of 4mol / hydrochloric acid aqueous solution, and reflux for 2 hours to obtain a mixture;

[0043] 2. Suction the mixture obtained above, wash the solid obtained by suction filtration with a large amount of deionized water until the filtrate is neutral, then wash the solid with acetone and ether, and finally place it in a vacuum drying oven at 25°C. Dry overnight at temperature;

[0044] 3. Take 450mg of the solid obtained in step 2 and disperse it in 25mL deionized water ultrasonically, add 288mg surfactant cetyltrimethylammonium chloride, 135mL absolute ethanol, 200mL deionized water, 2.5 mL of a mixed solution of saturated ammonia;

[0045] 4. Under the condition of stirring at 1500rpm, quickly add 225μL of 3,3'-bis(triethoxysilyl)-1,1'-biphenyl to the mixed solution obtained in step 3, and keep stirring for 8 hours After filtering, the obtai...

Example Embodiment

[0048] Example three

[0049] 1. Weigh 4g of silica gel balls with a particle diameter of 5mm and place them in an eggplant-shaped bottle, add 50mL of 4mol / hydrochloric acid aqueous solution, and reflux for 4 hours at room temperature to obtain a mixture;

[0050] 2. Suction the mixture obtained above, wash the solid obtained by suction filtration with a large amount of deionized water until the filtrate is neutral, then wash the solid with acetone and ether, and finally place it in a vacuum drying oven at 25°C. Dry overnight at temperature;

[0051] 3. Disperse 450 mg of the solid obtained in step 2 ultrasonically in 25 mL of deionized water, add 353 mg of surfactant octadecyl trimethyl ammonium bromide, 120 mL of anhydrous methanol, 200 mL of deionized water, 3.5 mL of a mixed solution of saturated ammonia;

[0052] 4. Under the stirring condition of rotation speed of 1500rpm, quickly add 242μL 1,4-bis(triethoxysilyl)benzene to the mixed solution obtained in step 3, keep stirring f...

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Abstract

The invention discloses a bonding type chromatographic column stationary phase and a preparation method thereof. Aryl bridged silsesquioxane is modified to the surface of a carrier silica gel by means of chemical bonding, the obtained chromatographic column stationary phase has a high specific surface area and narrow particle size distribution. The process route is simple, the raw materials are cheap and easily available, and the operation is convenient. Also, the chromatographic column stationary phase provided by the invention has a good separation effect on aryl compounds, and by changing different organic groups, different separation demands can be met.

Description

technical field [0001] The invention belongs to the field of chromatographic separation, and in particular relates to a bonded chromatographic column stationary phase and a preparation method thereof. Background technique [0002] High performance liquid chromatography is a modern column chromatography separation and analysis method developed on the basis of classical liquid chromatography by introducing the technology and theory of gas chromatography. Its analysis speed, separation efficiency and sensitivity are much higher than Classic liquid chromatography. The emergence of organic-inorganic hybrid silica has opened up a new development direction for chromatographic separation. Its advantage is that the polarity of the stationary phase can be adjusted by changing the organic part of the hybrid silica, covering from normal phase chromatographic columns to Reversed-phase chromatographic columns with different polarity fillers; in addition, the homogeneity and pore channels...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01J20/30B01D15/22
CPCB01D15/22B01J20/286B01J20/30B01J2220/54
Inventor 李艺杨永刚李宝宗侯逢文曹严方
Owner 上海熙华检测技术服务股份有限公司
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