Method for preparing high-purity pristimerin by high-speed countercurrent chromatography

[0017] 100 grams of dried root bark of Snakevine (produced in the southern mountainous area of ​​Hunan Province) was extracted by cold immersion in dichloromethane, each cold immersion was 24 hours, and then the solvent was recovered, and repeated three times to obtain a brown dry powdery substance, which is called crude extraction and drying. Object, accurately weigh 11.2 grams of dichloromethane rough extraction dry matter.

[0018] Accurately weigh 1 g of dichloromethane crude extraction dry matter, dissolve the sample with the upper phase of the solvent system of petroleum ether: ethanol: water (solvent volume ratio 10:10:1), turn on the constant temperature circulator, set the temperature to 25 degrees Celsius, and The upper phase of the solvent system is the stationary phase, and the lower phase is the mobile phase. The mobile phase (lower phase) and the stationary phase (upper phase) are pumped into the mobile phase (lower phase) and the stationary phase (upper phase) at th

[0020] Accurately weigh 1.2 grams of dichloromethane rough extraction dry matter, dissolve the sample with the upper phase of the solvent system of petroleum ether: ethanol: water (solvent volume ratio 10:9:1), turn on the constant temperature circulator, set the temperature to 24 degrees Celsius, and The upper phase of the solvent system is the stationary phase, and the lower phase is the mobile phase. The mobile phase (lower phase) and the stationary phase (upper phase) are pumped into the mobile phase (lower phase) and the stationary phase (upper phase) at the same time with double pumps. Phase, set the flow rate of the mobile phase to 1.8ml / min, turn on the host motor at the same time, adjust the speed to 860rpm, after ten minutes, the solvent system in the column reaches a dynamic equilibrium, and only the mobile phase flows out from the column outlet. Inject the sample through the injector, set the wavelength to 254nm, and the peak of priscarin appears about 295 minutes af

[0022]Accurately weigh 1.6 grams of dichloromethane rough extraction dry matter, dissolve the sample with the upper phase of the solvent system of petroleum ether: ethanol: water (solvent volume ratio 9:10:1), open the constant temperature circulator, set the temperature to 23 degrees Celsius, and The upper phase of the solvent system is the stationary phase, and the lower phase is the mobile phase. The mobile phase (lower phase) and the stationary phase (upper phase) are pumped into the mobile phase (lower phase) and the stationary phase (upper phase) at the same time with double pumps. Phase, set the flow rate of the mobile phase to 2.2ml / min, turn on the host motor at the same time, adjust the speed to 840rpm, after ten minutes, the solvent system in the column reaches a dynamic equilibrium, and only the mobile phase flows out from the column outlet. Inject the sample through the injector, set the wavelength to 254nm, and the peak of priscarin appears about 105 minutes after