Preparation method of Nudaphantin A
A technology of pumiladin and pumiladin, which is applied in the field of preparation of pubisin A, can solve the problems of less research on tannin and less pulicin A, and achieve large preparation volume, small sample loss, The effect of reducing the throughput
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Embodiment 1
[0020] Pulverize the rhizome of Pinnaea japonica, get 1kg, carry out ultrasonic extraction with 12kg75% ethanol solution, the ultrasonic frequency is 50KHz, extract 3 times, each time 0.5h, the extract is concentrated to obtain the ethanol crude extract of Pincus japonicus rhizome, use Ethyl acetate extracts the crude extract, filters, and concentrates the filtrate under reduced pressure to obtain a concentrated solution. After mixing the sample with a small amount of silica gel, the solvent is evaporated and put on a silica gel column. The dichloromethane-methanol ratio is 15:1, 7: 1. 2:1 gradient elution, TLC follow-up monitoring, collect the eluate of paciferin A, concentrate the eluent and inject it into a high-speed countercurrent chromatograph, and use cyclohexane-ethyl acetate-methanol-water 5:3:8 : 4 is a solvent system, the upper phase is a stationary phase, and the lower phase is a mobile phase, and the main engine rotating speed is 800rpm, and the flow rate of the mo...
Embodiment 2
[0022] Pulverize the rhizome of P. japonicum, take 1kg, carry out ultrasonic extraction with 10kg70% ethanol solution, the ultrasonic frequency is 45KHz, extract 2 times, each time 1.5h, the extract is concentrated, and obtain the ethanol crude extract of P. japonica rhizome, use The crude extract was extracted with ethyl acetate, filtered, and the filtrate was concentrated under reduced pressure to obtain a concentrated solution. After mixing the sample with a small amount of silica gel, the solvent was evaporated and put on a silica gel column. The dichloromethane-methanol ratio by volume was 17:1, 9: 1. 2:1 gradient elution, TLC follow-up monitoring, collect the eluate of paciferin A, concentrate the eluent and inject it into a high-speed countercurrent chromatograph, and use cyclohexane-ethyl acetate-methanol-water 3:2:6 : 4 is a solvent system, the upper phase is a stationary phase, and the lower phase is a mobile phase, the main engine rotating speed is 750rpm, and the fl...
Embodiment 3
[0024] Pulverize the rhizome of Pinnaea japonica, take 1kg, and carry out ultrasonic extraction with 8kg60% ethanol solution, the ultrasonic frequency is 70KHz, extract 2 times, each time for 1.5h, and concentrate the extract to obtain the crude ethanol extract of the rhizome of Pineapple japonica, use Ethyl acetate extracts the crude extract, filters, and concentrates the filtrate under reduced pressure to obtain a concentrated solution. After mixing the sample with a small amount of silica gel, the solvent is evaporated and put on a silica gel column. The dichloromethane-methanol ratio by volume is 16:1, 8: 1. 2:1 gradient elution, TLC follow-up monitoring, collect the eluate of paciferin A, concentrate the eluent and inject it into a high-speed countercurrent chromatograph, and use cyclohexane-ethyl acetate-methanol-water 3:2:6 : 2 is a solvent system, the upper phase is a stationary phase, and the lower phase is a mobile phase, and the rotating speed of the main engine is 7...
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