CN106727491A - A kind of Bilobanoate medicinal raw material - Google Patents
A kind of Bilobanoate medicinal raw material Download PDFInfo
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- CN106727491A CN106727491A CN201611119028.2A CN201611119028A CN106727491A CN 106727491 A CN106727491 A CN 106727491A CN 201611119028 A CN201611119028 A CN 201611119028A CN 106727491 A CN106727491 A CN 106727491A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
- A61K31/35—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom
- A61K31/352—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom condensed with carbocyclic rings, e.g. methantheline
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
- A61K31/365—Lactones
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/28—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
- C07D311/30—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only not hydrogenated in the hetero ring, e.g. flavones
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/12—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains three hetero rings
- C07D493/20—Spiro-condensed systems
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/22—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains four or more hetero rings
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Abstract
The invention discloses a kind of Bilobanoate medicinal raw material, belong to field of medicaments, including the flavones and lactone extracted from ginkgo, the flavones includes Quercetin, Kaempferol and Isorhamnetin；The lactone includes Bilobalide, ginkalide A, ginkolide B and ginkalide C；Wherein the ratio of flavones and lactone is 1：1.Bilobanoate medicinal raw material of the invention changes the standard of flavones and lactone ratio in original ginkgo biloba extract, it is determined that medicine has both removing free radical and the optimal ratio of anti-platelet aggregation.
Description
Technical field
The present invention relates to a kind of Bilobanoate medicinal raw material, belong to field of medicaments.
Background technology
Ginkgo biloba p.e has extensive pharmacological action, and its Total Ginkgo Flavone-Glycoides being rich in and Total Terpene Lactones are its hairs
Wave the topmost material base of such pharmacological action.And scavenging activated oxygen is anti-oxidant and antagonism platelet activating factor（PAF）
Anti-platelet aggregation is again the most prominent two pharmacological actions in its numerous bioactivity.East China Normal University's life science
Institute Chen Ji forces etc. once use highly sensitive chemoluminescence method experimental study, and " the natural flavonoid compound of 11 kinds of high-purities is clear
Except the structure-activity relationship of superoxide anion (O-2) ", and power to its activity sorted, it removes O-2 abilities
Size order is followed successively by：The new glycosides ＞ Quercetins ＞ rutin sophorins ＞ Hyperosides ＞ Kaempferols ＞ Radix Glycyrrhizaes of scutelloside ＞ wartwort
Chalcone ＞ aurantiamarin ＞ nevadensins, and river Chen Hebu A-grade in the first class c is invalid.Bilobalide-like substances can be with competitive antagonism
Platelet activating factor（PAF）So as to play powerful anti-platelet aggregation effect.Wherein with the ginkgo in ginkgo diterpenoid-lactone
Lactone B activity is most strong.And numerous studies data also indicates that the Flavonoid substances also activity with anti-platelet aggregation, ginkgolides
The class material also activity with scavenging activated oxygen, i.e. existed between two class materials intersect, complement each other etc. it is extremely multiple
Miscellaneous relation.Germany scientist once carried out comparison system, in-depth study to ginkgo biloba p.e（Plantation from ginkgo,
Supply, dwarfing, collection opportunity assurance, measure of active component enriching quantity of base fertilizer nutrition etc.）And formulated ginkgo biloba extract state
Border medicinal standard（General flavone >=24%, total lactones >=6%, ginkgoic acid ＜ 5ppm）.It is basis but this standard is relatively coarse
Extraction and preparation technique at that time and establish, rather than what is produced according to the good and bad assessment of pharmaceutical activity.In order to preferably play two
The pharmacological activity of effective constituents, reduces clinical administration dosage, further reduces insecurity and the interference of impurity band, probes into
Search out the more preferable proportionate relationship of two effective constituents and just seem necessary！Such research at present there is no and be found.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of Bilobanoate medicinal raw material, establishes the optimal of flavones and lactone
Ratio.
In order to solve the above technical problems, the technical solution used in the present invention is：
A kind of Bilobanoate medicinal raw material, including the flavones and lactone extracted from ginkgo, the flavones include Quercetin, kaempferia galamga
Phenol and Isorhamnetin；The lactone includes Bilobalide, ginkalide A, ginkolide B and ginkalide C；Wherein flavones and interior
The ratio of ester is 1：1.
Further improvement of the present invention is：The composition and ratio of weight and number of flavones be, 3 ~ 4 parts of Quercetin, Kaempferol 5 ~ 6
Part, 6 ~ 8 parts of Isorhamnetin.
Further improvement of the present invention is：The composition and ratio of weight and number of lactone be,
Bilobalide, 11 ~ 13 parts；Ginkalide A, 8 ~ 9 parts；Ginkolide B, 5 ~ 6 parts；Ginkalide C, 12 ~ 13 parts.
Further improvement of the present invention is：The extracting method of flavones is comprised the following steps,
Step A1, it is soluble in water to take a certain amount of ginkgo biloba p.e, supersonic oscillations dissolving is carried out at a temperature of 55 DEG C, afterwards
It is centrifuged, clear liquid is collected after filtering, the filter residue supersonic oscillations that repeat soluble in water are dissolved, is received after centrifugal filtration
Collection clear liquid, the clear liquid that will be collected twice merges, and obtains extract solution；
Step B1, the pH value of extract solution is adjusted to 4.5 ~ 5.0 with phosphoric acid,diluted or sodium hydroxide solution, then to addition etc. in extract solution
Have ethyl acetate and the n-butanol mixed liquor of volume are extracted, and extraction times are 3 times；The ethyl acetate and n-butanol mix
Ethyl acetate in liquid：The volume ratio of n-butanol is 4：1；
Step C1, extract is concentrated by evaporation, and the extract after concentration is carried out into freeze-drying, obtains Refined flavonoid powder.
Further improvement of the present invention is：The extracting method of lactone is comprised the following steps,
Step A2, it is soluble in water to take a certain amount of ginkgo biloba p.e, supersonic oscillations dissolving is carried out at a temperature of 55 DEG C, afterwards
It is centrifuged, clear liquid is collected after filtering, the filter residue supersonic oscillations that repeat soluble in water are dissolved, is received after centrifugal filtration
Collection clear liquid, the clear liquid that will be collected twice merges, and obtains extract solution；
Step B2, adjusts the pH value of extract solution to 4.5 ~ 5.0, with isometric ethyl acetate with phosphoric acid,diluted or sodium hydroxide solution
With petroleum ether extraction 2 ~ 6 times, ester obtains solid matter after mutually evaporating；
Step C2, solid matter is dissolved into its 20 times of water of volume, solution is centrifuged, filter after take supernatant liquor and add
Enter isometric ethyl acetate to extract 3 times, merge the solution of extraction, be concentrated by evaporation and reclaim volume, lactone is obtained after freeze-drying
CE；
, be dissolved in lactone CE in ethanol solution by heating water bath by step D2, and temperature naturally cools to room temperature, repeats
Heat, let cool and make crystal growth, be then placed within 4 DEG C of environment and be aged for lower 12 hours, mother liquor is separated, freeze-drying is obtained
Ginkgolides after exquisiteness.
Further improvement of the present invention is：Ethanol solution concentration in step D is 60%.
Due to using above-mentioned technical proposal, the beneficial effect produced by the present invention to be：
Bilobanoate medicinal raw material of the invention changes the standard of flavones and lactone ratio in original ginkgo biloba extract, it is determined that
Medicine has both removing free radical and the optimal ratio of anti-platelet aggregation, and the present invention is except with to god under ischemic, anaerobic condition
Outside through the protective effect of first cell and reparation injured neurons cell function, the Bilobalide institute of larger proportion is occupied in total lactones
The pharmacological action of the unique treatment alzheimer's disease having can also be highlighted.
Specific embodiment
The present invention is described in further details with reference to embodiment：
A kind of Bilobanoate medicinal raw material, including from ginkgo extract flavones and lactone, flavones include Quercetin, Kaempferol,
Isorhamnetin；The lactone includes Bilobalide, ginkalide A, ginkolide B, ginkalide C；Wherein flavones and lactone
Ratio is 1：1.
The composition and ratio of weight and number of flavones be, 3 ~ 4 parts of Quercetin, 5 ~ 6 parts of Kaempferol, 6 ~ 8 parts of Isorhamnetin.
The composition and ratio of weight and number of lactone be, Bilobalide, 11 ~ 13 parts；Ginkalide A, 8 ~ 9 parts；Ginkolide B, 5
~ 6 parts；Ginkalide C, 12 ~ 13 parts.
The extracting method of flavones is comprised the following steps,
Step A1, it is soluble in water to take a certain amount of ginkgo biloba p.e, supersonic oscillations is carried out at a temperature of 55 DEG C and dissolves 2 points
Clock, is centrifuged afterwards, and clear liquid is collected after filtering, the filter residue supersonic oscillations that repeat soluble in water is dissolved, 55
DEG C extract 15 minutes, clear liquid is collected after centrifugal filtration, the clear liquid that will collect twice merges, and obtains extract solution.
Step B1, adjusts the pH value of extract solution and adds to 4.5 ~ 5.0, then in extract solution with phosphoric acid,diluted or sodium hydroxide solution
Enter isometric have ethyl acetate and n-butanol mixed liquor to be extracted, extraction times are 3 times；Ethyl acetate and n-butanol mix
Ethyl acetate in liquid：The volume ratio of n-butanol is 4：1.
Step C1, extract is concentrated by evaporation, and the extract after concentration is carried out into freeze-drying, obtains Refined flavonoid powder.
The extracting method of lactone is comprised the following steps,
Step A2, it is soluble in water to take a certain amount of ginkgo biloba p.e, supersonic oscillations is carried out at a temperature of 55 DEG C and dissolves 2 points
Clock, is centrifuged afterwards, and clear liquid is collected after filtering, the filter residue supersonic oscillations that repeat soluble in water is dissolved, 55
DEG C extract 15 minutes, clear liquid is collected after centrifugal filtration, the clear liquid that will collect twice merges, and obtains extract solution.
Step B2, adjusts the pH value of extract solution to 4.5 ~ 5.0, with isometric acetic acid with phosphoric acid,diluted or sodium hydroxide solution
Ethyl ester and petroleum ether extraction 2 ~ 6 times, the ester of extraction obtains solid matter after pervaporation.
Step C2, solid matter is dissolved into its 20 times of water of volume, solution is centrifuged, filter after to take upper strata clear
Liquid adds isometric ethyl acetate to extract 3 times, merges the solution of extraction, is concentrated by evaporation and reclaims volume, is obtained after freeze-drying
Lactone CE.
, be dissolved in lactone CE in 60% ethanol solution by heating water bath by step D2, and temperature naturally cools to room
Temperature, repeats heating, lets cool and make crystal growth, is then placed within 4 DEG C of environment and is aged for lower 12 hours, and mother liquor is separated, cold
Jelly is dried to obtain the ginkgolides after exquisiteness.
Verified below by contrast experiment.
The ginkgo biloba extract that the ginkgo biloba extract that this experiment is used is produced for Zhejiang Kang Enbei companies, flavones therein and interior
The ratio of ester is the natural proportion of flavones and lactone in ginkgo.Extracted by the extracting method of above-mentioned flavones and lactone.
By the extracting method of above-mentioned flavones to article in flavones quality account for 51%-58%, without lactone；By lactone
Extracting method to article in lactone quality account for 37%-50%, containing having lacked flavones, the accounting of flavones quality for 8.0 ~
16.3%。
The flavones and lactone of extraction are carried out into mixing preparation according to actual content and goes out seven groups, flavones and lactone in each group
Ratio is respectively,
First group：Embodiment, flavones and lactone ratio are 1：1.Second group：Comparative example 1, flavones and lactone ratio are 4：1.3rd
Group：Comparative example 1, flavones and lactone ratio are 3：1.4th group：Comparative example 1, flavones and lactone ratio are 2：1.5th group：Contrast
Example 1, flavones and lactone ratio are 1：2.6th group：Comparative example 1, flavones and lactone ratio are 1：3.7th group：Comparative example 1, it is yellow
Ketone and lactone ratio are 1：4.
Tested one by one with two pharmacodynamics indexs of scavenging activated oxygen and anti-platelet aggregation respectively, and set negative and sun
Property control group.
Experiment one, scavenging activated oxygen experiment.
Using known strong reductant vitamin C（Sodium ascorbate）As positive control.Experiment sets three control comparisons groups,
Edaravone Injection, gingko leaf extract injection（Ginkgo Leaf Agent）And bilobalide injection（Hundred is abundant）, experimental technique is with confession
Test product, compares the scavenging ability of DPPH free radical of test sample and control comparisons product.Data are carried out using EXCEL and ORIGIN 8.0
Treatment and analysis, and carry out curve fitting, try to achieve EC50Concentration.
Experimental result is as follows, on the basis of general flavone glycoside concentration and converses the total extract test sample corresponding to the ratio
Concentration, is labeled as：General flavone glycoside concentration/total extract test sample concentration.Seven groups of EC of removing DPPH free radicals50Concentration is followed successively by
89.64 μ g.mL-1/337.58 μ g.mL-1,186.75 μ g.mL-1/443.63 μ g.mL-1,167.11 μ g.mL-1/425.45 μ
G.mL-1,138.99 μ g.mL-1/396.23 μ g.mL-1,67.11 μ g.mL-1/377.27 μ g.mL-1,50.02 μ g.mL-1/
410.74 μ g.mL-1,42.53 μ g.mL-1/376.87 μ g.mL-1.
Edaravone group EC in control comparisons group50Concentration is 86.88 μ g.mL-1；Gingko leaf extract injection（With ginkgo
Flavonoid glycoside concentration/total extract densimeter）EC50Concentration is 86.88 μ g.mL-1 and 157.10 μ g.mL-1/654.58 μ g.mL-
1；
Control comparisons product bilobalide injection stoste（Total lactones concentration is 5000 μ g.mL-1）Scavenging activity to DPPH is only
30.08%, do not obtain EC50Concentration.
Obtained as drawn a conclusion by experimental result.Under this experimental condition, experimental group 1 ~ 7 pair of removing of DPPH free radicals has
Effect property is set up.1 ~ 7 pair of DPPH radical scavenging activity of experimental group is obviously stronger than that bilobalide injection（Hundred is abundant）, test sample 1 ~
7 pairs of DPPH radicals scavenging EC50 total extract test sample concentrations are below gingko leaf extract injection（Ginkgo Leaf Agent）, for examination
The DPPH radicals scavenging EC50 total extracts test sample concentration of product 1 ~ 7 is all higher than Edaravone.
Be can be seen that from above-mentioned experiment：With general flavone：The change of total lactones ratio, extract Scavenging ability
Change therewith, i.e., required total extract test sample concentration value is different.Wherein especially with first group of embodiment（Flavones：Lactone=1:
1）In 1 ~ 7 group of test sample it is minimum to DPPH radicals scavenging EC50 total extract test sample concentration values（It is total Ginkgo Leaf Agent
The 337.58/654.58 ≈ 1/1.94 of extract concentrations, it is bilobalide injection（Hundred is abundant）337.58/5000 ≈ of total concentration
1/14.8）, i.e., this group Scavenging ability is most strong.
Experiment two, the experiment of anti-platelet aggregation screening active ingredients.
Using liquaemin as positive controls, with gingko leaf extract injection（Ginkgo Leaf Agent）And bilobalide injection
（Hundred is abundant）As control comparisons product, it is compared with total extract test sample.
Experimental technique is as follows, takes the qualified KM mouse 66 of quarantine, and 4 ~ 6 week old, hero female half and half is randomly divided into 11 by sex
Group（I.e. negative control group, positive controls, 1 group of test sample, 2 groups of test sample, 3 groups of test sample, 4 groups of test sample, 5 groups of test sample,
6 groups of test sample, 7 groups of test sample, 1 group of control comparisons product, 2 groups of control comparisons product）, every group 6.Using single tail vein injection side
Formula is administered, and 1 ~ 7 group of test sample gives test sample 1 ~ 7 successively, and 1 group of control comparisons product give Ginaton injection, control comparisons product 2
Group gives bilobalide injection, and dosage is 2.45mg/kg, and administration volume is 0.07 mL/10g, negative control group
The physiological saline of same volume is given, positive controls give same volume heparin sodium injection（Administration concentration is 1250 units/mL）.
10 minutes after administration, with the capillary for fractureing（About 1.5cm is long）A Inner corner of the eyes is carried out to mouse and takes blood, remove the 1st bleed after, carry
Drop 1 is bled on slide, immediately with manual time-keeping, is gently chosen 1 time to centre from drop of blood edge every 30s pins, when there is the trace of blood
Stop timing when provoking, and record the time, the as external clotting time.
Result of the test is with mean ± standard deviation（x±s）Represent, statistical procedures, each group and the moon are carried out using EXCEL softwares
Property control group between clotting time difference compared using paired-samples T-test, inspection level P values be 0.05.
In trial test and twice formal test, positive reference substance（Liquaemin）The all equal ＞ 600s of clotting time of mice of group,
Statistically significant is longer than negative control group, it is believed that this test method reliability.Result is summarized as follows：
Remarks：1：In terms of ginkgo biloba p.e, bilobalide injection group is to medicament for test sample 1 ~ 7 and the multigroup dosage of Jenner
Amount is in terms of ginkgolides；2：Liquaemin trial test dosage be 12500 units/kg, formal test dosage be 8750 units/
kg；
*：P ＜ 0.05；**：P ＜ 0.01.
Experiment conclusion：Under this experimental condition, the validity of experimental group 1 ~ 7 and control comparisons product extension clotting time of mice
Set up.Compared with negative controls, each test sample and control comparisons product can extend mouse under approximate Ginkgo Leaf Agent clinical dosage
Clotting time, and test sample 1,5 ~ 7 and bilobalide injection effect are better than Ginkgo Leaf Agent.In 1 ~ 7 group of test sample, consider and recognize
For 1 group of test sample（That is general flavone：Total lactones=1：1）Effect is optimal.
Be can be seen that from the experimental result tested twice.For radical scavenging activity：It is same to removing reaching
The EC of DPPH free radicals50Under the premise of concentration, the total extract test sample concentration required for test sample 1 ~ 7 is different, and concentration is got over
Small then Scavenging activity is stronger.Free radical experimental result is removed for the first time shows 1:Total extract test sample concentration required for 1 group
It is minimum.Remove free radical experimental result second and show 4：Total extract test sample concentration required for 1 group is minimum（Do not arrange
Except there is error in experiment）.
For anti-platelet aggregation activity：Under the conditions of identical administration concentration, in test sample 1 ~ 7 and Ginkgo Leaf Agent, ginkgo
Whose then anticoagulating active more long of external clotting time of ester injection is stronger.From trial test result, first time result of the test, second
Experimental result all shows 1:1 anti-coagulation activity is most strong.Comprehensive two test of pesticide effectiveness interpretations of result are assert：Flavones：Lactone=1:
1 group is to have both removing free radical and the optimal proportions of anti-platelet aggregation.Injected better than Ginkgo Leaf Agent and ginkgolides simultaneously
Liquid.
Claims (6)
1. a kind of Bilobanoate medicinal raw material, it is characterised in that including the flavones and lactone that are extracted from ginkgo, the flavones bag
Include Quercetin, Kaempferol and Isorhamnetin；The lactone includes Bilobalide, ginkalide A, ginkolide B and ginkgolides
C；Wherein the ratio of flavones and lactone is 1：1.
2. a kind of Bilobanoate medicinal raw material according to claim 1, it is characterised in that：The composition and parts by weight of flavones
Than being 3 ~ 4 parts of Quercetin, 5 ~ 6 parts of Kaempferol, 6 ~ 8 parts of Isorhamnetin.
3. a kind of Bilobanoate medicinal raw material according to claim 1, it is characterised in that：The composition and parts by weight of lactone
Than for,
Bilobalide, 11 ~ 13 parts；Ginkalide A, 8 ~ 9 parts；Ginkolide B, 5 ~ 6 parts；Ginkalide C, 12 ~ 13 parts.
4. a kind of Bilobanoate medicinal raw material according to claim 1 and 2, it is characterised in that：The extracting method bag of flavones
Include following steps,
Step A1, it is soluble in water to take a certain amount of ginkgo biloba p.e, supersonic oscillations dissolving is carried out at a temperature of 55 DEG C, afterwards
It is centrifuged, clear liquid is collected after filtering, the filter residue supersonic oscillations that repeat soluble in water are dissolved, is received after centrifugal filtration
Collection clear liquid, the clear liquid that will be collected twice merges, and obtains extract solution；
Step B1, the pH value of extract solution is adjusted to 4.5 ~ 5.0 with phosphoric acid,diluted or sodium hydroxide solution, then to addition etc. in extract solution
Have ethyl acetate and the n-butanol mixed liquor of volume are extracted, and extraction times are 3 times；The ethyl acetate and n-butanol mix
Ethyl acetate in liquid：The volume ratio of n-butanol is 4：1；
Step C1, extract is concentrated by evaporation, and the extract after concentration is carried out into freeze-drying, obtains Refined flavonoid powder.
5. a kind of Bilobanoate medicinal raw material according to claim 1 or 3, it is characterised in that：The extracting method bag of lactone
Include following steps,
Step A2, it is soluble in water to take a certain amount of ginkgo biloba p.e, supersonic oscillations dissolving is carried out at a temperature of 55 DEG C, afterwards
It is centrifuged, clear liquid is collected after filtering, the filter residue supersonic oscillations that repeat soluble in water are dissolved, is received after centrifugal filtration
Collection clear liquid, the clear liquid that will be collected twice merges, and obtains extract solution；
Step B2, the pH value of extract solution to 4.5 ~ 5.0 is adjusted with phosphoric acid,diluted or sodium hydroxide solution, with isometric
Ethyl acetate and petroleum ether extraction 2 ~ 6 times, the ester of extraction obtains solid matter after pervaporation；
Step C2, solid matter is dissolved into its 20 times of water of volume, solution is centrifuged, filter after take supernatant liquor and add
Enter isometric ethyl acetate to extract 3 times, merge the solution of extraction, be concentrated by evaporation and reclaim volume, lactone is obtained after freeze-drying
CE；
, be dissolved in lactone CE in ethanol solution by heating water bath by step D2, and temperature naturally cools to room temperature, repeats
Heat, let cool and make crystal growth, be then placed within 4 DEG C of environment and be aged for lower 12 hours, mother liquor is separated, freeze-drying is obtained
Ginkgolides after exquisiteness.
6. a kind of Bilobanoate medicinal raw material according to claim 5, it is characterised in that：Ethanol solution in step D is dense
Spend is 60%.
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| WO2019113861A1 (en) * | 2017-12-13 | 2019-06-20 | 巴卫松 | Ginkgo biloba extract medicinal raw material and preparation method therefor |
| CN110483447A (en) * | 2019-09-09 | 2019-11-22 | 南开大学 | 1 antagonist of Thyroid hormone receptor β and its application |
| WO2020037734A1 (en) * | 2018-08-20 | 2020-02-27 | 上海上药杏灵科技药业股份有限公司 | Ginkgo keto ester tablet and preparation method therefor |
| CN111166775A (en) * | 2020-02-24 | 2020-05-19 | 巴卫松 | Ginkgo leaf extract, ginkgo leaf extract medicament and application thereof |
| CN113730368A (en) * | 2021-09-30 | 2021-12-03 | 山东仁和制药有限公司 | A dripping pill containing ginkgolide and its preparation method |
| CN113730347A (en) * | 2021-09-30 | 2021-12-03 | 山东仁和制药有限公司 | Ginkgo diterpene lactone injection and preparation method thereof |
| CN115594654A (en) * | 2022-10-28 | 2023-01-13 | 河北荃美生物科技有限公司（Cn） | Extraction method and application of 7-demethyl ginkgetin and ginkgetin ester |
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| WO2019113861A1 (en) * | 2017-12-13 | 2019-06-20 | 巴卫松 | Ginkgo biloba extract medicinal raw material and preparation method therefor |
| CN110198713A (en) * | 2017-12-13 | 2019-09-03 | 巴卫松 | A kind of ginkgo biloba extract medicinal raw material and preparation method thereof |
| WO2020037734A1 (en) * | 2018-08-20 | 2020-02-27 | 上海上药杏灵科技药业股份有限公司 | Ginkgo keto ester tablet and preparation method therefor |
| EP3842054A4 (en) * | 2018-08-20 | 2021-11-17 | SPH Xing Ling Sci. & Tech. Pharmaceutical Co., Ltd. | Ginkgo keto ester tablet and preparation method therefor |
| CN110483447A (en) * | 2019-09-09 | 2019-11-22 | 南开大学 | 1 antagonist of Thyroid hormone receptor β and its application |
| CN111166775A (en) * | 2020-02-24 | 2020-05-19 | 巴卫松 | Ginkgo leaf extract, ginkgo leaf extract medicament and application thereof |
| CN113730368A (en) * | 2021-09-30 | 2021-12-03 | 山东仁和制药有限公司 | A dripping pill containing ginkgolide and its preparation method |
| CN113730347A (en) * | 2021-09-30 | 2021-12-03 | 山东仁和制药有限公司 | Ginkgo diterpene lactone injection and preparation method thereof |
| CN115594654A (en) * | 2022-10-28 | 2023-01-13 | 河北荃美生物科技有限公司（Cn） | Extraction method and application of 7-demethyl ginkgetin and ginkgetin ester |
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Application publication date: 20170531 |