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Preparation method of bilobalide B and bilobalide B prepared therefrom

A technology of ginkgolide and ginkgo biloba, which is applied in the field of natural medicinal chemistry, can solve the problems of high equipment requirements, no industrial application value, unsuitable for large-scale industrial production, and the like, and achieves the effect of improving safety.

Active Publication Date: 2015-08-05
BEIJING HANDIAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The content of Ginkgolide B in Ginkgo biloba is relatively low, about 0.2%, and the content in Ginkgo biloba extract is 1% to 2%, and the components of Ginkgo lactones have similar structures and small differences in properties. Therefore, from Ginkgo biloba, Separation of ginkgolide B from Ginkgo biloba extract is very difficult
There are many reports on the separation and purification of ginkgolide B, but most of them use organic solvents such as ethyl acetate, acetone, methanol, etc., which bring a lot of inconvenience and potential safety hazards to industrial production
[0004] Ginkgolide B separation and purification methods have been reported a lot, such as the methods mentioned in patents 200510063407.X, 200310104958, 200710050245.5, 200810046162.3, organic solvents are used in the separation and purification process, such as n-butanol, methyl alcohol, ethyl acetate, Normal hexane, and the yield of gained ginkgolide B is generally very low, and solvent consumption is bigger, does not have industrial application value; Again as the method mentioned in the patent 200910184916.6, with the total ginkgolide of purity > 95% as Raw materials, using recrystallization-supercritical CO 2 Extraction combination process is used for purification to obtain monomers GA and GB with a purity of >99.5%. This method has high requirements for starting materials and uses supercritical CO 2 Extraction requires high equipment; another example is patent 00117758.3, which uses preparative high performance liquid chromatography to separate and prepare GA and GB, and the liquid phase mobile phase is a mixture of ethyl acetate and petroleum ether, which is not suitable for large-scale industrial production

Method used

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  • Preparation method of bilobalide B and bilobalide B prepared therefrom
  • Preparation method of bilobalide B and bilobalide B prepared therefrom
  • Preparation method of bilobalide B and bilobalide B prepared therefrom

Examples

Experimental program
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Embodiment 1

[0041] Ginkgo biloba 150kg, pulverized, with 10 times (ratio of ethanol volume (ml) and ginkgo biloba weight (g), V / W) 70% ethanol heating reflux extraction 2 times, each time 2 hours, combined extracts, concentrated under reduced pressure at low temperature Until the ethanol is exhausted, and the volume of the concentrated solution reaches 4 times (ratio of ethanol volume (ml) to ginkgo leaf weight (g), V / W), store in 0°C-5°C for 24 hours, take it out, filter, slowly drop in the filtrate Add 95% ethanol until the alcohol concentration of the solution reaches 75%, refrigerate at 0°C-5°C for 24 hours, take it out, filter, concentrate until the ethanol is exhausted, add the filtrate to HPD450 macroporous resin column, first elute with pure water, and react with molish and thin-layer chromatography to control the elution end point, discard the eluent, and then elute with 70% ethanol, collect the eluent, concentrate, and dry to obtain 53.79 kg of Ginkgo biloba extract.

[0042] Ge...

Embodiment 2

[0046] Ginkgo biloba 150kg, pulverized, 8 times (ratio of ethanol volume (ml) and ginkgo biloba weight (g), V / W) 90% ethanol heating and reflux extraction 2 times, each time 2 hours, combined extracts, concentrated under reduced pressure at low temperature Until the ethanol is exhausted, and the volume of the concentrated solution reaches 3 times (ratio of ethanol volume (ml) to ginkgo leaf weight (g), V / W), store in 0°C-5°C for 24 hours, take it out, filter, slowly drop into the filtrate Add 95% ethanol until the alcohol concentration of the solution reaches 75%, refrigerate at 0°C-5°C for 24 hours, take it out, filter, concentrate until the ethanol is exhausted, add the filtrate to a DM130 macroporous resin column, first elute with pure water, and react with molish and thin-layer chromatography to control the elution endpoint, discard the eluent, and then elute with 60% ethanol, collect the eluent, concentrate, and dry to obtain 57.34 kg of Ginkgo biloba extract.

[0047] Ge...

Embodiment 3

[0051] Ginkgo biloba 150kg, pulverized, 12 times (ratio of ethanol volume (ml) to ginkgo biloba weight (g), V / W) 50% ethanol heating and reflux extraction 1 time, 2 hours each time, combined extracts, concentrated under reduced pressure at low temperature Until the ethanol is exhausted, and the volume of the concentrated solution reaches 5 times (ratio of ethanol volume (ml) to ginkgo leaf weight (g), V / W), store in 0°C-5°C for 12 hours, take it out, filter, slowly drop in the filtrate Add 95% ethanol until the alcohol concentration of the solution reaches 75%, refrigerate at 0°C-5°C for 12 hours, take it out, filter, concentrate until the ethanol is exhausted, add the filtrate to HPD700 macroporous resin column, first elute with pure water, and react with molish and thin-layer chromatography to control the elution end point, discard the eluate, and then elute with 80% ethanol, collect the eluate, concentrate, and dry to obtain 60.56 kg of Ginkgo biloba extract.

[0052] Get G...

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Abstract

The invention provides a preparation method of bilobalide B and the bilobalide B prepared therefrom. In the preparation method of the bilobalide B, the toxic organic solvent is replaced with ethyl alcohol and water in association with separation column, aqueous processing and recrystallization of ethyl alcohol of low and intermediate concentrations, so as to separate and purify the bilobalide B, thereby obtaining the bilobalide B of a high purity, with few impurity content, and without bilobalide as well as allergenic component ginkgolic acid.

Description

technical field [0001] The invention belongs to the field of natural medicinal chemistry, and in particular relates to a preparation method of ginkgolide B and the prepared ginkgolide B. Background technique [0002] Ginkgolides belong to terpenoids and are an important active ingredient in Ginkgo biloba. They all have the effect of antagonizing platelet activating factor (PAF) receptors, glycine (Gly) receptors, and γ-aminobutyric acid (GABA) receptors. , wherein the antagonism of PAF receptors is manifested as highly selective antagonism of platelet aggregation induced by PAF, thereby preventing the formation of thrombus, and the antagonism of Gly receptors and GABA receptors is a protective effect on the central nervous system; antagonism of PAF receptors Bioactivity studies have shown that ginkgolide B (GB) has the strongest activity, followed by ginkgolide A (GA), then ginkgolide C, and finally ginkgolide M (only present in ginkgo root bark, leaves not included). [0...

Claims

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Application Information

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IPC IPC(8): C07D493/22
CPCC07D493/22
Inventor 林德良
Owner BEIJING HANDIAN PHARMA
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