Preparation method of corilagin
A supercritical, pore adsorption technology, applied in the preparation of sugar derivatives, chemical instruments and methods, production of bulk chemicals, etc., can solve problems such as the lack of reports on large-scale industrial production and preparation of high-purity corylazine, and achieve the benefits of large-scale production. Production operation, less pollution and less energy consumption
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Embodiment 1
[0026] Get phylloxera coarse powder 10Kg, join in CO 2 In the supercritical extractor, ethyl acetate is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 3%, the extraction pressure is 10MPa, the temperature is 35°C, and the CO 2 Flow rate 1ml / g crude drug min, extraction time 80min, get extract, add water to dissolve, filter, filtrate is adsorbed by HPD700 type macroporous adsorption resin, 20% ethanol is eluted, collects the eluent of 3 times of column volume, reduces Recover ethanol under pressure and concentrate, add acetic acid to the concentrated solution to adjust the pH to 4-4.5, carry out 6-stage countercurrent extraction with ethyl acetate-water mixed solvent with a ratio of 10:2, the volume ratio of the concentrated solution to the total amount of mixed solvent is 1: 6. Combine the extracts, recover the solvent under reduced pressure, add absolute ethanol to crystallize, separate the crystals, wash, and dry to obtain...
Embodiment 2
[0028] Get phylloxera coarse powder 10Kg, join in CO 2 In the supercritical extractor, ethyl acetate is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 8%, the extraction pressure is 30MPa, the temperature is 55°C, and the CO 2 Flow rate 3ml / g crude drug min, extraction time 150min, get extract, add water to dissolve, filter, filtrate is adsorbed by H50 type macroporous adsorption resin, eluted with 60% ethanol, collects the eluate of 8 times of column volume, reduces Recover ethanol under pressure and concentrate, add acetic acid to the concentrated solution to adjust the pH to 4-4.5, carry out 10-stage countercurrent extraction with ethyl acetate-water mixed solvent with a ratio of 10:2, the volume ratio of the concentrated solution to the total amount of mixed solvent is 1: 10. Combine the extracts, recover the solvent under reduced pressure, add absolute ethanol to crystallize, separate the crystals, wash, and dry to obta...
Embodiment 3
[0030] Get phylloxera coarse powder 10Kg, join in CO 2 In the supercritical extractor, ethyl acetate is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 5%, the extraction pressure is 20MPa, the temperature is 45°C, and the CO 2 Flow rate 2ml / g crude drug min, extraction time 100min, get extract, add water to dissolve, filter, filtrate is absorbed by AB8 type macroporous adsorption resin, 40% ethanol elutes, collects the eluent of 5 times of column volume, reduces Recover ethanol under pressure and concentrate, add acetic acid to the concentrated solution to adjust the pH to 4-4.5, carry out 8-stage countercurrent extraction with ethyl acetate-water mixed solvent with a ratio of 10:2, the volume ratio of the concentrated solution to the total amount of mixed solvent is 1: 8. Combine the extracts, recover the solvent under reduced pressure, add absolute ethanol to crystallize, separate the crystals, wash, and dry to obtain 12.4...
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