Bilobalide B raw material and preparation thereof
A ginkgolide and raw material technology, applied in the field of ginkgolide B raw material and its preparation, can solve the problems of less than 2%, low transfer rate, difficult to form industrialization, etc., and achieve cost saving, simple process and low cost Effect
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Embodiment 1
[0032] Weigh 10 kg of ginkgo leaves, add 500L of 1% hydrochloric acid and soak for 30 minutes, filter to obtain 480L of soaking liquid, extract with 2400L of n-butanol, concentrate the extract to an appropriate amount, add an appropriate amount of 100-200 mesh silica gel, mix and dry, Go up silica gel column (diameter-to-height ratio is 1: 1, silica gel consumption 3kg), with ethyl acetate: acetone is the ratio preparation mobile phase of 4: 6, control flow rate 180ml / min, collect the 40L effluent containing ginkgolide B, Concentrate and dry to obtain 6g of dry cream, add 180ml of 95% ethanol to crystallize, and obtain 2.3g of ginkgolide B raw material, wherein, the content of ginkgolide B is 91.5%.
Embodiment 2
[0034] Weigh 20kg of ginkgo leaves, add 700L of 0.5% hydrochloric acid and soak for 150min, filter to obtain 650L of filtrate, extract with 1300L of acetone, concentrate the extract to an appropriate amount, add an appropriate amount of 100-200 mesh silica gel, mix and dry, and put on a silica gel column (diameter-to-height ratio is 1: 1, silica gel consumption 5.7kg), with ethyl acetate: sherwood oil is the ratio preparation mobile phase of 7: 3, control flow rate 410ml / min, collect 70L effluent, concentrate and dry to obtain 10g dry paste, Add 300ml of 95% ethanol to crystallize to obtain 4.1g of ginkgolide B raw material, wherein the content of ginkgolide B is 92.0%.
Embodiment 3
[0036] Weigh 1kg of Ginkgo biloba extract (in line with the requirements of "Chinese Pharmacopoeia" 2000 edition, Taiyuan Xingyuan Biochemical Co., Ltd.), add 5L of 0.1% hydrochloric acid and soak for 60min, filter to obtain 4.8L of filtrate, and extract with 9.6L of ethyl acetate , concentrate the extract to an appropriate amount, add an appropriate amount of 100-200 mesh silica gel, mix and dry, put on a silica gel column (the ratio of diameter to height is 1:1, and the amount of silica gel is 2.5kg), with n-butanol:petroleum ether as 8:2 Prepare the mobile phase according to the ratio, control the flow rate of 360ml / min, collect 35L of the effluent, concentrate and dry to obtain 5g of dry cream, add 150ml of 95% ethanol to crystallize, and obtain 1.7g of ginkgolide B raw material, wherein the content of ginkgolide B is 90.7% .
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