A kind of refining method of ginkgolide a and ginkgolide b
A technology of ginkgolide and a refining method, applied in the direction of organic chemistry and the like, can solve the problems of low utilization rate of raw materials, difficult to realize industrialization, easy pollution of the environment, etc., and achieve great application value, improve utilization efficiency, and high product purity. Effect
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Embodiment 1
[0034] Take 1000g of ginkgo biloba extract extract, dilute it to 0.5g crude drug / mL with aqueous solution, add 1000ml ethyl acetate for extraction, extract three times in total, combine the ethyl acetate extract, concentrate under reduced pressure at 45°C until there is no solvent, add 10 % ethanol to make the concentration of the concentrated solution 0.5g / mL, wet-pack the column, let the liquid pass through the MCI resin, first use 30% ethanol to elute the resin to remove impurities, and elute 3BV in total. The elution rate was 1BV / h, and then the resin was eluted with 40% ethanol at the same flow rate, and the first 2BV eluate and the last 2BV eluate were collected respectively, concentrated under reduced pressure at 45°C to 1g / ml extract, and 500ml80 % ethanol, heated at 70°C until dissolved, left standing in the refrigerator at 4°C for 24h to crystallize, after the crystals were precipitated, filtered with suction to obtain the crude products of ginkgolide A and ginkgolide...
Embodiment 2
[0036]Get 500g of ginkgo biloba extract extract, dilute to 0.2g / mL with aqueous solution, add 1000ml ethyl acetate to extract, extract altogether four times, combine ethyl acetate extract, mother liquor and extract after crystallization in embodiment 1 are combined Concentrate the combined solution under reduced pressure at 45°C until there is no solvent, add 240ml of 20% ethanol to make the concentration of the concentrated solution 0.5g / mL, wet-pack the column, let the drug solution pass through the MCI resin, first elute the resin with 30% ethanol to remove impurities, To remove water-soluble and polar impurities, elute 4BV in total, the elution rate is 2BV / h, then use 40% ethanol to elute the resin at the same flow rate, take the first 2BV eluate and the last 3BV eluate respectively, respectively After concentrating under reduced pressure at 45°C to no solvent, add 800ml of 70% ethanol, heat to dissolve at 70°C, and stand in a refrigerator at 4°C for 12 hours to crystallize...
Embodiment 3
[0038] Get 800g of ginkgo biloba extract extract, dilute to 0.4g / mL with aqueous solution, add 4000ml ethyl acetate to extract, extract altogether five times, combine ethyl acetate extract, the mother liquor and extract after crystallization in embodiment 2 are combined , concentrated under reduced pressure at 45°C until there is no solvent, added 350ml of 20% ethanol to make the concentration of the concentrated solution 0.5g / mL, wet-packed the column, made the liquid pass through the MCI resin, and first eluted the resin with 30% ethanol to remove impurities. Remove water-soluble and highly polar impurities, elute 4BV in total, and the elution rate is 1BV / h, then use 40% ethanol to elute the resin at the same flow rate, take the first 2BV eluate and the last 3BV eluate, respectively, in After concentrating under reduced pressure at 45°C until there is no solvent, add 500ml of 60% ethanol, heat to dissolve at 70°C, and stand in the refrigerator at 4°C for 24 hours to crystalli...
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