Preparation method of siliceous inorganic flavonoid molecular engram microsphere

A technology of molecularly imprinted microspheres and flavonoids, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of uneven flow distribution of mobile phase, small specific surface area, limited adsorption capacity, etc., and achieve good selective adsorption and separation ability. , The preparation process is simple, and the physical and chemical properties are good.

Inactive Publication Date: 2007-02-28
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of the functional monomers and crosslinking agents used in molecular imprinting technology are organic compounds such as acrylate, chitosan, cellulose, etc., and the prepared materials are mostly organic materials, and the preparation process of organic materials is complicated. Solvents are easy to swell
At present, some people have also prepared silica inorganic molecularly imprinted polymers by the sol-gel method. This material has good stability and a large selective adsorption capacity. However, due to its irregular shape, fragments are easily generated during the adsorption process. If it is used for chromatography Or the separation column packing is likely to cause problems such as unstable column pressure and uneven distribution of mobile phase flow; at the same time, due to the relatively small specific surface area, the size of the adsorption capacity is also limited

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Embodiment 1: under the condition of 70 ℃ water bath, add 0.03 g of luteolin into a 250 mL three-necked flask, dissolve with 50 mL of ethanol; then add 3 mL of aminopropyltriethoxysilane to the flask, and reflux for 8 After 1 hour, get solution a; also under the condition of 70 ℃ water bath, mix 9 mL of ethyl orthosilicate, 50 mL of 98% ethanol, 50 mL of deionized water and 2 mL of Span 20, and add ammonia water to adjust the pH value to 10 to catalyze the reaction, After the reaction was carried out for 1 hour, solution a was added, and the reaction was continued for 5 hours; the hydrolyzed product was filtered through filter paper, and the filter cake was placed in an oven at 85 ° C for drying for 48 hours to obtain 3 g of product; 3 g of product was added to a Soxhlet Ethanol was heated and refluxed for 10 hours to remove surfactants and templates; finally, the product was dried at 85°C to obtain siliceous molecularly imprinted microspheres.

[0011] The adsorption e...

Embodiment 2

[0012] Example 2: Under the condition of water bath at 70°C, 0.05g of puerarin was added to a 250mL three-necked flask, and dissolved in 50mL of ethanol; then 3mL of aminopropyltriethoxysilane was added to the flask, and the reaction was refluxed for 8 hours. Then, solution a was obtained; also under the condition of water bath at 70°C, 9mL of ethyl orthosilicate, 50mL of 98% ethanol, 50mL of water and 2mL of Span 20 were mixed and stirred evenly, and ammonia water was added to adjust the pH value to 10 to catalyze the reaction; the reaction was carried out for 1 hour Then add solution a, continue the reaction for 5 hours and stop; filter the hydrolyzate with filter paper, put it in an oven for drying at 85°C for 48 hours to obtain 3g of molecularly imprinted microspheres; then take 3g of the dried material and put it into a Soxhlet extractor , extracted with 300 mL of 98% ethanol under reflux for 10 hours to remove surfactants and templates. Finally, the product is obtained a...

Embodiment 3

[0013] Embodiment 3: under the condition of 70 ℃ water bath, add 0.03g of catechin into a 250mL three-necked flask, dissolve it with 50mL of ethanol; then add 3mL of aminopropyltriethoxysilane to the flask, reflux reaction 8 After 1 hour, get solution a; also under the condition of 70 ℃ water bath, mix and stir 9 mL of ethyl orthosilicate, 50 mL of 98% ethanol, 50 mL of water and 2 mL of Span 20, and add ammonia water to adjust the pH value to 10 to catalyze the reaction; the reaction is carried out for 1 After 1 hour, solution a was added, and the reaction was continued for 5 hours to stop. The hydrolyzed product was filtered with filter paper and dried in an oven at 85° C. for 48 hours to obtain 3 g of product, which was loaded into a Soxhlet extractor and extracted with 300 mL of ethanol under reflux for 10 hours to remove surfactant and template. Finally, the siliceous molecularly imprinted microspheres are obtained after the product. The results of the same adsorption ex...

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Abstract

The invention discloses a preparing method of silicon inorganic flavone molecular imprinting microballoon in the separating purifying domain, which comprises the following steps: blending certain density mold agent solution and functional monomer according to rate; adding and refluxing to obtain former solution; blending ethyl silicate, alcohol, water and face activator evenly; adding ammonia to do catalytic reaction; adding former solution after reacting for a certain time; hydrolyzing for certain time continuously; filtering the hydrolytic product; drying in the sorbitic extractor; extracting through alcohol for a long time; drying again to obtain the product.

Description

technical field [0001] The invention relates to a preparation method of siliceous inorganic molecularly imprinted microspheres with specific selective adsorption to natural product flavonoid molecules. The invention belongs to the preparation technology of materials for separating and purifying flavonoids. Background technique [0002] Flavonoids are a class of natural products that widely exist in nature. It is estimated that about 20% of Chinese herbal medicines contain flavonoids, which shows that they are rich in resources. Studies have shown that flavonoids have a variety of biological activities, in addition to using their antibacterial, anti-inflammatory, anti-mutation, antihypertensive, heat-clearing and detoxifying, sedative, diuretic and other effects, in anti-oxidation, anti-cancer, anti-cancer, inhibiting lipase, etc. There are also significant effects. Because of these biological activities of flavonoids, the research of flavonoids has entered a new stage, whi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/04B01J20/14
Inventor 张裕卿秦震
Owner TIANJIN UNIV
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