Preparation method of licochalcone A
A technology of licorice chalcone and licorice, which is applied in the field of preparation of licorice chalcone A, to achieve the effects of large-scale production operation, low energy consumption and low pollution
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Embodiment 1
[0024] Get licorice (derived from the dry root and rhizome of Glycyrrhiza uralensis Fisch. of the leguminous plant Glycyrrhiza uralensis Fisch.) 10Kg, pulverize, add to CO 2 In the supercritical extractor, ethanol is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 2%, the extraction pressure is 10MPa, the temperature is 50°C, and the CO 2 The flow rate is 1ml / g crude drug·min, the extraction time is 80min, and the extract is obtained, which is added to the polyamide chromatographic column of nylon 66 and eluted with a mixed solvent of ethanol and water at a ratio of 2:1 as the eluent. The amide film is developed with the above eluent as a supporting test, and the fraction corresponding to Rf=5-5.5 on the polyamide film is collected, the solvent is recovered, acetone is added to crystallize, washed and dried to obtain yellow needle crystals - licochalcone A66.5g, detected by HPLC, the purity is 92.5%, UV, IR, MS, 2 HNMR, 13 ...
Embodiment 2
[0026] Get licorice (derived from the dry root and rhizome of Glycyrrhiza inflata Bat. of the leguminous plant Glycyrrhiza inflata Bat.) 10Kg, pulverize, join in CO 2 In the supercritical extractor, ethanol is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 4%, the extraction pressure is 30MPa, the temperature is 70°C, and the CO 2 The flow rate is 3ml / g crude drug·min, the extraction time is 120min, and the extract is obtained, which is added to the chromatographic column of nylon 6 polyamide and eluted with ethanol-water mixed solvent with a ratio of 2:1 as eluent. The polyamide film is developed with the above eluent as a supporting test, collect the fraction corresponding to Rf=5-5.5 on the polyamide film, recover the solvent, add acetone to crystallize, wash and dry to obtain yellow needle crystals-licorice chal Ketone A56.2g, detected by HPLC, the purity is 94.8%, UV, IR, MS, 2 HNMR, 13 The data characterizing its phy...
Embodiment 3
[0028] Get 10Kg of licorice (derived from the dry root and rhizome of the leguminous plant Glycyrrhiza glabra L.), pulverize it, and add it to CO 2 In the supercritical extractor, ethanol is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 3%, the extraction pressure is 20MPa, the temperature is 65°C, and the CO 2 The flow rate is 2ml / g crude drug·min, the extraction time is 100min, and the extract is obtained, which is added to the chromatographic column of nylon 66 polyamide, eluted with ethanol-water mixed solvent with a ratio of 2:1 as the eluent, and the same kind of The polyamide film is developed with the above eluent as a supporting test, collect the fraction corresponding to Rf=5-5.5 on the polyamide film, recover the solvent, add acetone to crystallize, wash and dry to obtain yellow needle crystals-licorice chal Ketone A73.2g, detected by HPLC, the purity is 95.9%, UV, IR, MS, 2 HNMR, 13 The data characterizing its...
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