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Porous silica gel microsphere surface tripterygium wilfordii extract molecularly imprinted polymer and preparation and application thereof

A technology of porous silica gel and molecular imprinting, applied in other chemical processes, chemical instruments and methods, etc., can solve problems such as tailing, low resolution, broadening of chromatographic peaks, etc.

Inactive Publication Date: 2015-04-29
BEIJING FORESTRY UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Early molecularly imprinted polymers are usually in the form of lumps, which are obtained after grinding and sieving. The particles are irregular and non-uniform in size. When they are used for chromatographic separation, the resolution is low, and it is easy to cause broadening of chromatographic peaks and severe tailing.
Less selectivity when used in solid phase extraction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1 Preparation Example of Triptolide Molecularly Imprinted Polymer

[0023] (1) Modification of porous silica microspheres by vinyltrimethoxysilane

[0024] Add 10 g of porous silica gel microspheres to 50 mL of a mixed solution of hydrochloric acid / deionized water with a volume ratio of 1:1, heat and stir to reflux for 8 h, then let stand overnight, cool to room temperature, remove the hydrochloric acid solution by suction filtration, and use The silica gel was rinsed repeatedly with deionized water, and then washed with an appropriate amount of ethanol. The silica gel was collected and dried in vacuum. The dried silica gel was activated at 200 °C for 12 h. Weigh 8 g of activated silica gel into a flask, add 50 mL of toluene, 5 mL of vinyltrimethoxysilane, 3 mL of pyridine, and 1 mL of triethylamine, stir and mix evenly, then pass through nitrogen to remove oxygen for 30 minutes, seal it, and React at 80°C for 16 h. After the reaction, the reaction liquid w...

Embodiment 2

[0027] Example 2 Preparation Example of Triptolide Molecularly Imprinted Polymer

[0028] (1) Modification of porous silica gel by γ-methacryloxypropyltrimethoxysilane

[0029] Add 10 g of porous silica gel microspheres to 50 mL of a mixed solution of nitric acid / deionized water with a volume ratio of 1:1, heat and stir to reflux for 8 h, then let stand overnight, cool to room temperature, remove the hydrochloric acid solution by suction filtration, and use The silica gel was rinsed repeatedly with deionized water, and then washed with an appropriate amount of ethanol. The silica gel was collected and dried in vacuum. The dried silica gel was activated at 180 °C for 16 h. Weigh 5 g of activated silica gel into a flask, add 40 mL of toluene, 3 mL of γ-methacryloxypropyltrimethoxysilane, and 0.5 mL of triethylamine, stir and mix evenly, and then pass through nitrogen to remove oxygen for 30 minutes , sealed, stirred (300 rpm), and reacted at 82°C for 20 h. After the reacti...

Embodiment 3

[0032] Example 3 Preparation example of tripterine molecularly imprinted polymer

[0033] (1) Modification of porous silica gel microspheres: same as Example 1 (1).

[0034] (2) Preparation of tripterine molecularly imprinted polymer on the surface of silica gel

[0035] Add 0.1 mmol of triptolide and 0.6 mmol of 4-vinylpyridine into 22 mL of toluene, stir for 10 min, and then let stand at room temperature for 8 h to allow the functional monomer methacrylic acid and the template molecule triptolide to form super Molecular complex, then add 2.1 mmol ethylene glycol dimethacrylate to the system, 1 g vinyltrimethoxysilane-modified silica gel, ultrasonic for 12 min, add azobisisobutyronitrile, and blow nitrogen to remove oxygen 30 min, sealed, and reacted at 60 °C for 24 h. After the reaction, the surface imprinted silica gel was washed with acetone and toluene, and then eluted with ethanol-acetic acid solution to remove the template molecule tripterine, then the imprinted sili...

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PUM

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Abstract

The invention discloses a porous silica gel microsphere surface tripterygium wilfordii extract molecularly imprinted polymer and preparation and application thereof. The invention relates to a tripterygium wilfordii extract molecularly imprinted polymer. In a pore-forming solvent, under the action of a crosslinking agent, by using a tripterygium wilfordii extract as a template molecule and using vinylpyridine, methylpropenoic acid or acrylamide and the like as a functional monomer, a grafting action is performed on the surface of a porous silica gel microsphere to obtain the surface molecularly imported polymer using the porous microsphere as a matrix. The tripterygium wilfordii extract molecularly imprinted polymer provided by the invention has high preferential adsorption capability for the template molecule tripterygium wilfordii extract and has good stability.

Description

technical field [0001] The invention relates to the fields of functional polymer materials, biochemical separation and analytical chemistry. More specifically, it relates to a molecularly imprinted polymer of Tripterygium wilfordii extract on the surface of porous silica gel microspheres. [0002] The invention also relates to a preparation method of the tripterygium wilfordii extract molecularly imprinted polymer on the surface of the porous silica gel microsphere. [0003] The invention also relates to the application of the tripterygium wilfordii extract molecularly imprinted polymer on the surface of the porous silica gel microsphere. Background technique [0004] Tripterygium wilfordii Hook.f. is a woody vine of the genus Tripterygium in the family Euonymus. It is also known as Huangteng, Huangtengmu, Huanglateng, etc. It is distributed in the south of the Yangtze River Basin and Southwest China. Tripterygium wilfordii, as a traditional Chinese medicine, is bitter in ...

Claims

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Application Information

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IPC IPC(8): C08F292/00C08F222/14C08F220/06C08F226/06C08J9/26C08J9/28B01J20/26B01J20/285B01J20/30
Inventor 雷建都何静刘静王璐莹邓立红戴林
Owner BEIJING FORESTRY UNIVERSITY
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