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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

AI Technical Summary

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 existing silica gel stationary phase modification process is relatively complicated, with small specific surface area, weak pertinence, and less stable in medium

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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Effect test

Embodiment 1

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

[0035] 2. Suction filter 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 solid with acetone and ether respectively, and finally place it in a vacuum drying oven, at room temperature dry overnight;

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

[0037] 4. Quickly add 225 μL of 4,4'-bis(triethoxysilyl)-1,1'-biphenyl to the mixed solution obtained in step 3 under the stirring condition of 1500rmp, and keep sti...

Embodiment 2

[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 filter 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 respectively, and finally place it in a vacuum drying oven at 25°C Dry overnight at room temperature;

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

[0045] 4. Quickly add 225 μL of 3,3'-bis(triethoxysilyl)-1,1'-biphenyl to the mixed solution obtained in step 3 under the stirring condition of 1500rmp, and keep stirring for 8 hours After...

Embodiment 3

[0049] 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 at room temperature for 4 hours to obtain a mixture;

[0050] 2. Suction filter 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 respectively, and finally place it in a vacuum drying oven at 25°C Dry overnight at room temperature;

[0051] 3. Ultrasonically disperse 450 mg of the solid obtained in step 2 in 25 mL of deionized water, and add 353 mg of surfactant octadecyltrimethylammonium bromide, 120 mL of anhydrous methanol, 200 mL of deionized water, and 3.5 In the mixed solution of mL saturated ammonia water;

[0052] 4. Quickly add 242 μL of 1,4-bis(triethoxysilyl)benzene to the mixed solution obtained in step 3 under the stirring condition of 1500 rpm, keep stirr...

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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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