Preparation method of carissone
A technology of fake tiger ketone and magnesium oxide, which is applied in the field of natural medicinal chemistry to achieve the effects of fast separation speed, simple operation and large processing capacity
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Embodiment 1
[0023] Grind the leaves of Akniga branchiae, take 1kg and put it into a supercritical extraction kettle, and feed it with liquid CO 2 , set the extraction pressure to 25MPa, and the temperature to 40°C. After reaching the above parameters, adjust the liquid CO 2 The flow rate is 4ml / g crude drug / min, 95% ethanol solution is used as entrainer, the amount of entrainer is 15% of the total extraction solvent, dynamic extraction is carried out for 50min, analysis is carried out at a pressure of 7.5MPa and a temperature of 40°C, and the obtained extract is dissolved in methanol , add a small amount of neutral magnesia to mix the sample, evaporate the solvent, put it on the magnesia column by dry method, gradient elution with petroleum ether-acetone 23:3, 15:3, 5:3, 2:3 mixed solvent, collect the eluate Concentrate under reduced pressure to obtain crude extract. Take petroleum ether, ethyl acetate, methanol, and water and mix according to 6:8:7:5. After mixing and layering, take the...
Embodiment 2
[0025] Grind the leaves of Aknegia chinensis, take 2kg and add it to a supercritical extraction kettle, and feed it with liquid CO 2 , set the extraction pressure to 35MPa, and the temperature to 50°C. After reaching the above parameters, adjust the liquid CO 2 The flow rate is 5ml / g crude drug / min, 99% ethanol solution is the entrainer, the entrainer dosage is 18% of the total extraction solvent, dynamic extraction is carried out for 70min, and the analysis is carried out at a pressure of 9MPa and a temperature of 32°C. After the obtained extract is dissolved in methanol, Add a small amount of neutral magnesia to mix the sample, evaporate the solvent, put it on the magnesia column by dry method, and elute with petroleum ether-acetone 21:3, 12:3, 5:3, 2:3 mixed solvent gradient elution, collect the eluate and reduce Concentrate under reduced pressure to obtain a crude extract. Take petroleum ether, ethyl acetate, methanol, and water and mix according to 7:5:6:4. After mixing ...
Embodiment 3
[0027] Grind the leaves of Aknegia chinensis, take 2kg and add it to a supercritical extraction kettle, and feed it with liquid CO 2 , set the extraction pressure to 30MPa and the temperature to 55°C. After reaching the above parameters, adjust the liquid CO 2 The flow rate is 2.5ml / g crude drug / min, 100% ethanol solution is used as entrainer, the entrainer dosage is 12% of the total extraction solvent, dynamic extraction is carried out for 90min, analysis is carried out at a pressure of 8MPa and a temperature of 35°C, and the obtained extract is dissolved in methanol , add a small amount of neutral magnesia to mix the sample, evaporate the solvent, put it on the magnesia column by dry method, gradient elution with petroleum ether-acetone 18:3, 9:3, 2:3 mixed solvent, collect the eluate and concentrate under reduced pressure to obtain crude extract. Take petroleum ether, ethyl acetate, methanol, and water and mix according to 5:7:8:7. After mixing and layering, take the upper...
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