Method for extracting dehydrated vinblastine and epoxy vinblastine from fresh grass of catharanthus roseus
A technology for dehydrating vinblastine and epoxy vinblastine, which is applied in the direction of organic chemistry and the like, can solve the problems of affecting extraction sufficiency, being unsuitable for mass production, and low in safety, and achieves low cost, easy large-scale industrial production, and production technology. simple effect
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Embodiment 1
[0025] Take 100 kilograms of fresh periwinkle flowers, beat and pulverize them, soak them in 0.5% sulfuric acid solution twice, and soak them for 4 hours each time. Combine the soaking solution, adjust the pH value of the soaking solution to 2, pass through the cation exchange resin HD-8 at 4 times the bed volume / hour, weak acid macroporous type, column diameter ratio 8:1, and wash with water until it is colorless. Soak with 4% ammonium chloride and 3% ethanol solution for 4 hours. Elute with 2% sodium hydroxide and 5% ethanol, detect the appearance of alkaloids by TLC, and start collecting. Combine and concentrate for treatment, extract and alkalize the solution and evaporate to dryness and separate by silica gel chromatography to obtain 40 grams of alkaloids, including 1.14 grams of vinblastine, 0.08 grams of vincristine, 0.65 grams of dehydrated vinblastine, 0.63 grams of epoxy vinblastine, and 0.63 grams of vinblastine. 3.24 grams of alkali and 3.20 grams of Wen Duoling. ...
Embodiment 2
[0027] Take 100 kg of fresh periwinkle flowers, beat and pulverize them, soak and extract them twice with 0.5% sulfuric acid solution. Soak for 4 hours each time. Combine the soaking solution and adjust the pH value of the soaking solution to 3. Pass through cation exchange resin D61, sodium type, column diameter ratio 8:1 at 4 times bed volume / hour, and elute with water until colorless. Soak with 4% sodium chloride and 2% ethanol solution for 4 hours. Elute with 3% sodium hydroxide and 10% ethanol, detect the appearance of alkaloids by TLC, and start collecting. Combine and concentrate for treatment, extract and alkalize the liquid and evaporate to dryness and separate by silica gel chromatography to obtain 40 grams of alkaloids, including 1.15 grams of vinblastine, 0.08 grams of vincristine, 0.68 grams of dehydrated vinblastine, 0.68 grams of epoxy vinblastine, and 0.68 grams of vinblastine. Alkali 3.47 grams, Wen Duoling 3.71 grams.
Embodiment 3
[0029] Take 100 kg of fresh periwinkle flowers, beat and pulverize them, soak and extract them twice with 0.5% sulfuric acid solution. Soak for 6 hours each time. Combine the soaking solution and adjust the pH value of the soaking solution to 4. Pass through cation exchange resin D61 at 4 times bed volume / hour, hydrogen type, column diameter ratio 7:1, eluted with water until colorless. Then soak in 6% ammonium chloride 2% ethanol for 4 hours. Elute with 3% ammonium hydroxide and 22% ethanol, detect the appearance of alkaloids by TLC, and start to collect. Combine and concentrate for treatment, extract and alkalize the solution and evaporate to dryness and separate by silica gel chromatography to obtain 40 grams of alkaloids, including 1.53 grams of vinblastine, 0.09 grams of vincristine, 0.78 grams of dehydrated vinblastine, 0.75 grams of epoxy vinblastine, and 0.75 grams of vinblastine. 3.48 grams of alkali and 3.72 grams of Wen Duolin.
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