Bilobalide extraction and purification process
A ginkgolide and process technology, applied in the field of traditional Chinese medicine pharmacy, can solve the problems that scientific research, production and application cannot be satisfied, the cost of ginkgolide process is high, the content of ginkgolide is low, etc., and the cost is low, the price is low, and the operation is simple. Effect
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Embodiment 1
[0025] Weigh 200 grams of ginkgo leaves and pulverize them, add 80% ethanol to reflux and extract 3 times, the amount of ethanol each time is 8 times of the weight of the medicinal material, and the reflux time is 2 hours each time. Combine the extracts for 3 times, recover ethanol until there is no alcohol smell, degrease with gasoline 5 times, extract the water phase with butanone 5 times, combine the butanone solution, wash with saturated lime water and remove impurities, recover the butanone solution, and obtain Ginkgo biloba The crude ester was recrystallized with 40% ethanol solution, allowed to stand, filtered, and dried at 90°C to obtain the refined product of ginkgolide.
[0026] It has been determined that the transfer rate of ginkgolides is over 60%, the total content of ginkgolides A, B, C and bilobalide is over 92%, of which the content of ginkgolide B is over 40%, and the main impurity, ginkgolic acid, is less than 100%. 2 out of 10,000.
Embodiment 2
[0028] Weigh 200 grams of ginkgo leaves and pulverize them, add 70% ethanol to reflux and extract 3 times, the amount of ethanol each time is 7 times the weight of the medicinal material, and the reflux time is 2.5, 2.5, 2 hours respectively. Combine the extracts for 3 times, recover ethanol until there is no alcohol smell, degrease with carbon tetrachloride for 5 times, extract the water phase with ether for 6 times, combine the ether solution, wash with 0.4% borax aqueous solution and remove impurities, recover ether, and obtain ginkgolide The crude product was recrystallized with 50% ethanol solution, allowed to stand, filtered, and dried at 90°C to obtain the refined product of ginkgolide.
[0029] It has been determined that the transfer rate of ginkgolides is over 60%, the total content of ginkgolides A, B, C and bilobalide is over 92%, of which the content of ginkgolide B is over 40%, and the main impurity, ginkgolic acid, is less than 100%. 2 out of 10,000.
Embodiment 3
[0031] Weigh 200 grams of Ginkgo biloba leaves and pulverize them, add 10% methanol for warm soaking and extracting 3 times, the amount of methanol each time is 10 times of the weight of the medicinal material, and warm soaking time is 5 hours each time. Combine the extracts for 3 times, recover methanol, degrease with carbon tetrachloride 5 times, extract the water phase with ether 6 times, combine the ether solution, wash with 0.5% potassium bicarbonate solution to remove impurities, recover ether, and obtain crude ginkgolide , recrystallized with 70% ethanol solution, allowed to stand, filtered, and dried at 80°C to obtain refined ginkgolide.
[0032] It has been determined that the transfer rate of ginkgolides is over 60%, the total content of ginkgolides A, B, C and bilobalide is over 92%, of which the content of ginkgolide B is over 40%, and the main impurity, ginkgolic acid, is less than 100%. 2 out of 10,000.
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