Preparation method of nudaphantin
A bamboo and herbal technology, applied in the direction of organic chemistry, etc., can solve the problems of no bamboo herbal extraction process, less bamboo herbs, etc., and achieve the effects of large preparation amount, small sample loss, and reduced processing capacity.
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Embodiment 1
[0017] Grind the rhizome of bamboo grass, take 1kg, and carry out ultrasonic extraction with 12kg of 75% ethanol solution. Extract the crude extract with ethyl ester, filter, and concentrate the filtrate under reduced pressure to obtain a concentrated solution. After mixing the sample with a small amount of polyamide resin, evaporate the solvent, put it on a polyamide resin column, and use dichloromethane-methanol at a volume ratio of 10:1 , 6:1, 1:1 gradient elution, TLC follow-up monitoring, collect the eluate of bamboo plant, concentrate the eluent and inject it into a high-speed countercurrent chromatograph, and use cyclohexane-ethyl acetate-methanol-water 5:3 :8:4 is the solvent system, the upper phase is the stationary phase, the lower phase is the mobile phase, the speed of the main engine is 800rpm, and the flow rate of the mobile phase is 3ml / min. According to the detector spectrum, the fractions of bamboo grass are collected, concentrated, and freeze-dried That is, 1...
Embodiment 2
[0019] Grind the rhizome of bamboo grass, take 1kg, and carry out ultrasonic extraction with 10kg of 70% ethanol solution, the ultrasonic frequency is 25-40KHz, extract twice, each time for 1.5h, the extract is concentrated and dried, and the ethanol crude extract of the rhizome of bamboo grass is obtained, Extract the crude extract with ethyl acetate, filter, and concentrate the filtrate under reduced pressure to obtain a concentrated solution. After mixing the sample with a small amount of polyamide resin, evaporate the solvent and put it on a polyamide resin column. :1, 5:1, 1:1 gradient elution, TLC follow-up monitoring, collect the eluate of bamboo plant, concentrate the eluate and inject it into the high-speed countercurrent chromatograph, and use cyclohexane-ethyl acetate-methanol-water 5 :5:8:4 is the solvent system, the upper phase is the stationary phase, the lower phase is the mobile phase, the speed of the main engine is 750rpm, and the flow rate of the mobile phase...
Embodiment 3
[0021] Grind the rhizome of bamboo grass, take 1kg, and use 8kg of 60% ethanol solution for ultrasonic extraction, the ultrasonic frequency is 40KHz, extract twice, each time for 1.5h, the extract is concentrated and dried to obtain the ethanol crude extract of bamboo grass rhizome, and use acetic acid Extract the crude extract with ethyl ester, filter, and concentrate the filtrate under reduced pressure to obtain a concentrated solution. After mixing the sample with a small amount of polyamide resin, evaporate the solvent, put it on a polyamide resin column, and use dichloromethane-methanol at a volume ratio of 10:1 , 5:1, 1:1 gradient elution, TLC follow-up monitoring, collect the eluate of bamboo plant, concentrate the eluent and inject it into a high-speed countercurrent chromatograph, and use cyclohexane-ethyl acetate-methanol-water 3:2 :6:2 is the solvent system, the upper phase is the stationary phase, the lower phase is the mobile phase, the speed of the main engine is ...
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