Method for preparing high-purity rhynchophylline monomer
An urticine and high-purity technology, which is applied in the field of preparation of high-purity urticine monomers, can solve problems such as uricine monomers that have not yet been seen, and achieves a separation environment with ease, short separation time and high recovery rate. Effect
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Embodiment 1
[0028] Weigh 10 kg of Uncaria vine, coarsely crush it, and carry out reflux extraction with 95% ethanol solution in mass percent concentration. The number of extractions is 3 times, and each extraction is 2 hours. The 3 extractions are combined and concentrated under reduced pressure to obtain an extract. The extract was dissolved in 1000 milliliters of water, the pH value was adjusted to 9.5 with ammonia water, and then extracted with chloroform. After the chloroform extract was concentrated, 42.6 g of Uncaria uncaria extract was obtained.
[0029] The rhynchophylline extract was loaded on the silica gel column chromatography, and the chloroform-methanol ratio was 50:1, 30:1, 20:1, 10:1 to elute successively according to the volume ratio, and the eluate was collected and subtracted. Concentrate under pressure to get crude rhynchophylline;
[0030] According to the volume ratio, take petroleum ether: ethyl acetate: isopropanol: water as 2:6:3:9 to measure each solvent, after m...
Embodiment 2
[0034] Weigh 10 kg of Uncaria vine, coarsely crush it, and carry out reflux extraction with 90% ethanol solution in mass percent concentration. The number of extractions is 2 times, and each extraction is 3 hours. The 2 extractions are combined and concentrated under reduced pressure to obtain an extract. The extract was dissolved in 1000 milliliters of water, the pH was adjusted to 10 with ammonia water, and then extracted with chloroform. After the chloroform extract was concentrated, 44.3 g of Uncaria uncaria extract was obtained.
[0035] The rhynchophylline extract is loaded on a silica gel column chromatography, and the chloroform-methanol ratio is 20:1 for elution according to the volume ratio, the eluate is collected, concentrated under reduced pressure, and the crude rhynchophylline is obtained;
[0036] According to the volume ratio, take petroleum ether: ethyl acetate: ethanol: water as 2:7:2:9 to measure each solvent, after mixing, take 10mL of mixed separation solv...
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