Preparation method for polyphenol monomers from gnaphlium affine
A polyphenolic compound, the technology of Shamrock, which is applied in the field of preparation of polyphenolic compound monomers in Shamrock, can solve the problem of less research on compounds, and achieve the effect of simple method, simple method operation, and high purity
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Embodiment 1
[0018] A method for preparing polyphenolic compound monomers in Shamrock, the steps are:
[0019] (1) Fresh sage grass is dried in an oven at 60°C and crushed to 10 meshes, then the pulverized raw material is added with 20 times the amount of sage grass powder and ethanol with a mass concentration of 50%, and refluxed at 70°C Extract for 0.5h, filter, repeat the extraction of the filter residue once, combine the extracts and concentrate under reduced pressure until there is no ethanol smell, and at the same time adjust the pH = 3 with hydrochloric acid, filter to remove the precipitate, pass the filtrate through the layer containing D101 resin at a flow rate of 4BV / h Column analysis, the volume of the upper column is 0.5h after adsorption, washed with water until colorless, then eluted with 4BV mass concentration of 60% ethanol at a flow rate of 2BV / h, collected ethanol eluate, concentrated under reduced pressure and freeze-dried , to obtain the purified product of sagebrush t...
Embodiment 2
[0023] (1) Fresh sagebrush is dried in an oven at 60°C and crushed to 10 meshes, then the pulverized raw material is added with 25 times the amount of sagebrush powder and ethanol with a mass concentration of 60%, and refluxed at 75°C Extract for 1 hour, filter, and repeat the extraction of the filter residue once, combine the extracts and concentrate under reduced pressure until there is no ethanol smell, and at the same time adjust the pH to 3 with hydrochloric acid, filter to remove the precipitate, and pass the filtrate through the chromatography equipped with D101 resin at a flow rate of 4BV / h Column, the upper column volume is 0.5h after adsorption, washed with water until colorless, then eluted with 5BV mass concentration of 60% ethanol at a flow rate of 3BV / h, collected the ethanol eluate, concentrated under reduced pressure and freeze-dried. Obtain the product of sagebrush through the column purification;
[0024](2) Fully mix n-hexane, ethyl acetate, methanol, and gl...
Embodiment 3
[0027] (1) Fresh sage grass is dried in an oven at 60°C and crushed to 20 meshes, then the pulverized raw material is added with 30 times the amount of sage grass powder and ethanol with a mass concentration of 70%, and refluxed at 80°C Extract for 1 hour, filter, and repeat the extraction of the filter residue once, combine the extracts and concentrate under reduced pressure until there is no ethanol smell, and at the same time adjust the pH to 3 with hydrochloric acid, filter to remove the precipitate, and pass the filtrate through the chromatography equipped with D101 resin at a flow rate of 4BV / h Column, the upper column volume is 0.5h after adsorption, washed with water until colorless, and then eluted with 6BV mass concentration of 60% ethanol at a flow rate of 4BV / h, collected ethanol eluate, concentrated under reduced pressure and freeze-dried. Obtain the product of sagebrush through the column purification;
[0028] (2) Fully mix n-hexane, ethyl acetate, methanol, and...
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