Preparation method of nectandrine B

[0019] The bark of Phoebe phoenix is ​​crushed, and 1kg is added to a supercritical extraction kettle, and liquid CO 2 , set the extraction pressure to 25MPa, and the temperature to 45°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 12% of the total extraction solvent, dynamic extraction is carried out for 90min, and the analysis is carried out at a pressure of 7MPa and a temperature of 40°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 20:3, 12:3, 5:3 mixed solvent gradient, collect the eluate and concentrate under reduced pressure to obtain crude Extract. Take n-hexane, ethyl acetate, methanol, and water and mix them according to 7:9:4:5. After mixing and layering, take the upper ph...

[0021] The bark of Phoebe phoenix is ​​crushed, and 2kg is added to a supercritical extraction kettle, and liquid CO 2 , set the extraction pressure to 20MPa, and the temperature to 50°C. After reaching the above parameters, adjust the liquid CO 2 The flow rate is 3ml / g crude drug / min, 95% ethanol solution is used as entrainer, and the amount of entrainer is 18% of the total extraction solvent. Dynamic extraction is carried out for 50 minutes, analyzed at a pressure of 9MPa and a temperature of 35°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 gradient elution with petroleum ether-acetone 18:3, 10:3, 5:3 mixed solvent, collect the eluate and concentrate under reduced pressure to obtain crude Extract. Take n-hexane, ethyl acetate, methanol, and water and mix according to 5:8:3:4. After mixing and layering, take the upper phase and fill the ...

[0023] The bark of Phoebe phoenix is ​​crushed, and 2kg is added to a supercritical extraction kettle, and liquid CO 2 , set the extraction pressure to 32MPa, and the temperature to 60°C. After reaching the above parameters, adjust the liquid CO 2 The flow rate is 5ml / g crude drug / min, 95% ethanol solution is used as entrainer, and the amount of entrainer is 16% of the total extraction solvent. Dynamic extraction is carried out for 80 minutes, analyzed at a pressure of 8MPa and a temperature of 30°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, gradient elution with petroleum ether-acetone 17:3, 9:3, 5:3 mixed solvent, collect the eluate and concentrate under reduced pressure to obtain crude Extract. Take n-hexane, ethyl acetate, methanol, and water and mix them according to 4:7:5:3. After mixing and layering, take the upper phase and fill the ...