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.
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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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