CN1173724C - Systemic separation process and prepn of ginkgetin, ginkgolide and bilobalide - Google Patents
Systemic separation process and prepn of ginkgetin, ginkgolide and bilobalide Download PDFInfo
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- CN1173724C CN1173724C CNB011198249A CN01119824A CN1173724C CN 1173724 C CN1173724 C CN 1173724C CN B011198249 A CNB011198249 A CN B011198249A CN 01119824 A CN01119824 A CN 01119824A CN 1173724 C CN1173724 C CN 1173724C
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Abstract
The present invention discloses a systemic separation method of ginkgo leaf extract, and a preparation of the extract obtained by the method. By the systemic separation method, more than 50% of gingko total flavonoids, more than 98% of gingko lactone B, and more than 98.5% of bilobalide are obtained.
Description
The present invention relates to a kind of preparation method and preparation thereof of Folium Ginkgo extract, particularly relate to the system's separation method and the preparation thereof of ginkgetin, bilobalide, bilobalide.
The system of Folium Ginkgo total flavones, ginkalide B, bilobalide separates and formulation method
The a lot of documents of the extracting method of Folium Ginkgo all have report, and decoction and alcohol sedimentation technique, Amberlyst process are arranged, and the content of the effective site ginkgetin that is extracted is about 20%.The Folium Ginkgo chemical constituent mainly contains Ginkgo total flavones, bilobalide (wherein the strongest with the ginkalide B activity) and bilobalide.Three kinds of composition drug effects have nothing in common with each other.Existing gingko leaf preparation adopts the mixture of Semen Ginkgo extrac more.
The object of the invention is to provide a kind of system's extraction separation method of using, and obtains above-mentioned three kinds of compositions, Folium Ginkgo total flavones＞50%, ginkalide B＞95%, bilobalide＞95%; And the medicament of the Folium Ginkgo extract preparation that obtains with this method.
The present invention seeks to realize like this: ginkgo leaf powder is broken into coarse powder (crossing 20 mesh sieves), boils three times with the aqueous solution that contains 1-2% antioxidant, each water consumption be 10-15 doubly, each time is 1-2 hour.Three times the water extract merges, and filters, and filtrate is at first passed through the polyamide adsorption column, and the medicinal liquid of holding back after the absorption of polyamide column adsorption column is standby; Polyamide column triplication water washing, reuse 60-90% ethanol elution, eluent is used the n-hexane extraction secondary after concentrating, and concentrates, and drying promptly gets Folium Ginkgo total flavones.
The medicinal liquid of holding back after the absorption of polyamide column adsorption column is crossed macroporous adsorptive resins, uses the triplication water washing, the alcohol desorption of reuse 60-90%, and eluent concentrates, and uses ethyl acetate extraction three times, collects the ethyl acetate part, and concentrate drying gets Ginkgo total lactones.
Total lactone is mixed sample with silica gel 1-2 weight portion, and last silicagel column separates, and uses the chloroform-methanol gradient elution, gets bilobalide and ginkgolectone AB.
Bilobalide gets colourless bilobalide through recrystallization, and content is 98.0%.
Ginkgolectone AB gets ginkalide B through recrystallization repeatedly, and content is 98.5%.
The post height of the macroporous resin adsorption post in this method, polyamide column, silicagel column is 4-15 with column diameter ratio, and optimum ratio is 4; Be best with 70% ethanol elution respectively during two kinds of adsorption column desorbings; Macroporous resin adsorption post model can be commercially available DHP100, D101, AB-8, WLD, D141 etc.; Antioxidant can be vitamin C, sodium sulfite, and sodium pyrosulfite, antioxidant concentration of aqueous solution can be 0.5%.
Can make Folium Ginkgo total flavones capsule or acceptable clinically medicament with the Ginkgo total flavones that said method obtains.
With the ginkalide B that said method obtains, can make injection or any acceptable forms clinically.
With the bilobalide that said method obtains, can make injection or any clinical acceptable forms.
The extract that makes with the inventive method shows Ginkgo total flavones content＞50% after testing, ginkgoic acid content＜5ppm; The bilobalide yield is 0.045, content 98.0%; Ginkalide B yield 0.015%, content 98.5%.
Testing result sees Table:
| Title | Content (%) | |||||
| The HPLC method | Colorimetry | |||||
| 1 batch | 2 batches | 3 batches | 4 batches | 5 batches | 6 batches | |
| Ginkgo total flavones | 48.19 | 49.8 | 46.1 | 58.5 | 59.9 | 55.2 |
| Ginkalide B | 93.85 | 90.13 | 95.85 | - | - | - |
| Bilobalide | 95.86 | 96.72 | 96.10 | - | - | - |
With three kinds of medicaments that Folium Ginkgo extract is made that said method obtains, constant product quality is easily controlled, and effective component content is single in the medicine surveys, the purity height.The clinical efficacy of Ginkgo total flavones is well known, and comprises improving cerebrovascular and peripheral vessel blood circulation effectively, is used for arteriosclerosis, hypertension, diseases such as apoplexy; The clinical efficacy of ginkalide B is well known, and comprises having neuroprotective and edema effect, is used for the treatment of nervous system disease, encephalopathy and myelopathy, hypomnesis, alzheimer disease etc.; The clinical efficacy of bilobalide also is known to the public, comprises the anti-platelet aggregation factor, is specificity PAF antagonist, is used for diseases such as prevention and treatment arteriosclerosis, allergic asthma, bronchospasm, transplant rejection, shock.
Embodiment 1:
Folium Ginkgo coarse powder (crossing 20 mesh sieves) 100g adds 0.5% sodium metabisulfite solution 1200,1000,1000ml respectively, and heated and boiled stirs and extracts three times.For the first time, extracted 1.5 hours; For the second time, extracted 1 hour; For the third time, extracted 1 hour.Go medicinal residues to merge three medicinal liquids, filter, cross the polyamide adsorption column, the medicinal liquid of after the absorption of polyamide adsorption column, holding back, standby; Polyamide column 3000ml water washing, reuse 70% ethanol elution, eluent is used the n-hexane extraction secondary after concentrating, and concentrates, and drying promptly gets Folium Ginkgo total flavones.The medicinal liquid of holding back after the absorption of polyamide column adsorption column is crossed macroporous adsorptive resins DHP100, uses the 3000ml water washing, the alcohol desorption of reuse 70%, and eluent concentrates, and uses ethyl acetate extraction three times, collects the ethyl acetate part, and concentrate drying gets Ginkgo total lactones; Total lactone is mixed sample with silica gel 1.5 grams, and last silicagel column separates, and uses the chloroform-methanol gradient elution, gets bilobalide and ginkgolectone AB;
Bilobalide gets colourless bilobalide through recrystallization, and the bilobalide yield is 0.045%, and content is 98.0%; Ginkgolectone AB gets ginkalide B through recrystallization repeatedly, and the bilobalide yield is 0.015%, and content is 98.5%.
Embodiment 2:
10 kilograms of Folium Ginkgo coarse powder add 0.5% vitamin c solution 120L, 100L, 100L respectively, and heated and boiled stirs and extracts three times.For the first time, extract 90min; For the second time, extract 60min; For the third time, extract 60min, go medicinal residues to merge three medicinal liquids, filter, cross the polyamide adsorption column, the medicinal liquid of after the absorption of polyamide adsorption column, holding back, standby; Polyamide column triplication water washing, reuse 75% ethanol elution, eluent is used the n-hexane extraction secondary after concentrating, and concentrates, and drying promptly gets ginkgetin 134.64g, yield 1.35%, content 48.19% (HPLC method), 55% (colorimetry).Get Folium Ginkgo total flavones (extract) 20g, medical starch 230g, mixing is granulated, and 1000 capsules are adorned in oven dry, and every capsules contains the Folium Ginkgo total flavones must not be lower than 10mg.
Embodiment 3:
10 kilograms of Folium Ginkgo coarse powder add 0.6% vitamin c solution 120L, 100L, 100L respectively, and heated and boiled stirs and extracts three times.For the first time, extract 90min; For the second time, extract 60min; For the third time, extract 60min, go medicinal residues to merge three medicinal liquids, filter, cross the polyamide adsorption column, the medicinal liquid of holding back after the absorption of polyamide adsorption column is crossed macroporous adsorptive resins D141, use the triplication water washing, the alcohol desorption of reuse 80%, eluent concentrates, and uses ethyl acetate extraction three times, collect the ethyl acetate part, concentrate drying gets Ginkgo total lactones; Total lactone is mixed sample with silica gel 150 grams, and last silicagel column separates, and uses the chloroform-methanol gradient elution, gets bilobalide and ginkgolectone AB; Bilobalide gets colourless bilobalide 4.5 grams through recrystallization, and yield is 0.045%, and content is 98.0%.
Get bilobalide 0.25g, sodium chloride (injection) 9g, water for injection adds to 1000ml.
Take by weighing bilobalide and sodium chloride for injection by recipe quantity, add the injection water, heating slightly, stirring and dissolving, filtration, the filtrate fill, sealing by fusing, sterilization is promptly.The every 2ml of this product includes bilobalide 0.5mg.
Embodiment 4:
10 kilograms of Folium Ginkgo coarse powder add 0.8% sodium sulfite solution 120L, 100L, 100L respectively, and heated and boiled stirs and extracts three times.For the first time, extract 90min; For the second time, extract 60min; For the third time, extract 60min, go medicinal residues to merge three medicinal liquids, filter, cross the polyamide adsorption column, the medicinal liquid of holding back after the absorption of polyamide adsorption column is crossed macroporous adsorptive resins AB-8, use the triplication water washing, the alcohol desorption of reuse 65%, eluent concentrates, and uses ethyl acetate extraction three times, collect the ethyl acetate part, concentrate drying gets Ginkgo total lactones; Total lactone is mixed sample with silica gel 150 grams, and last silicagel column separates, and uses the chloroform-methanol gradient elution, gets bilobalide and ginkgolectone AB; Bilobalide AB gets ginkalide B 1.5g through recrystallization, yield 0.015%, content 98.5% (HPLC normalization method).
Get ginkalide B 0.5g, sodium chloride (injection) 9g, water for injection adds to 1000ml
Method for making: take by weighing ginkalide B, sodium chloride for injection by recipe quantity, add the injection water, heating slightly, stirring and dissolving filters, the filtrate fill, sealing by fusing, sterilization is promptly.The every 2ml of this product includes ginkalide B 1.0mg.
Fig. 1 is a system of the present invention extraction and separation process flow chart.
Claims (6)
1, a kind of system's separation method that extracts Folium Ginkgo extract, it is characterized in that this method is: Folium Ginkgo coarse powder 100 weight portions, the aqueous solution of the 1-2% antioxidant of doubly measuring with 10-15, heated and boiled, stirring are extracted three times respectively, and each extraction time is 1-2 hour, go medicinal residues to merge three medicinal liquids, filter, cross the polyamide column adsorption column, the medicinal liquid of after the absorption of polyamide column adsorption column, holding back, standby; Polyamide column triplication water washing, reuse 60-90% ethanol elution, eluent is used the n-hexane extraction secondary after concentrating, and concentrates, and drying promptly gets Folium Ginkgo total flavones;
The medicinal liquid of holding back after the absorption of polyamide column adsorption column is crossed macroporous adsorptive resins, uses the triplication water washing, the alcohol desorption of reuse 60-90%, and eluent concentrates, and uses ethyl acetate extraction three times, collects the ethyl acetate part, and concentrate drying gets Ginkgo total lactones;
Total lactone is mixed sample with silica gel 1-2 weight portion, and last silicagel column separates, and uses the chloroform-methanol gradient elution, gets bilobalide and ginkgolectone AB;
Bilobalide gets colourless bilobalide through recrystallization;
Ginkgolectone AB gets ginkalide B through recrystallization repeatedly.
2, a kind of extracting method of ginkgetin, it is characterized in that this method is: the aqueous solution of the 1-2% antioxidant that the Folium Ginkgo coarse powder is doubly measured with 10-15, heating is boiled heat, is stirred and extract three times respectively, each extraction time is 1-2 hour, go medicinal residues to merge three medicinal liquids, filter, cross the polyamide adsorption column, the medicinal liquid of after the absorption of polyamide adsorption column, holding back, standby; Polyamide column triplication water washing, reuse 60-90% ethanol elution, eluent is used the n-hexane extraction secondary after concentrating, and concentrates, and drying promptly gets Folium Ginkgo total flavones.
3, a kind of extracting method of bilobalide, it is characterized in that this method is: the aqueous solution of the 1-2% antioxidant that Folium Ginkgo coarse powder 10-15 doubly measures, heated and boiled, stirring are extracted three times respectively, each extraction time is 1-2 hour, go medicinal residues to merge three medicinal liquids, filter, cross the polyamide adsorption column, the medicinal liquid of holding back after the absorption of polyamide adsorption column is crossed macroporous absorption power fat post DHP100, use the triplication water washing, the alcohol desorption of reuse 60-90%, eluent concentrates, and uses ethyl acetate extraction three times, collect the ethyl acetate part, concentrate drying gets Ginkgo total lactones;
Total lactone is mixed sample with silica gel 1-2 weight portion, and last silicagel column separates, and uses the chloroform-methanol gradient elution, gets bilobalide and ginkgolectone AB;
Bilobalide gets colourless bilobalide through recrystallization.
4, a kind of extracting method that extracts ginkalide B, it is characterized in that this method is: the aqueous solution of the 1-2% antioxidant that the Folium Ginkgo coarse powder is doubly measured with 10-15, heated and boiled, stirring are extracted three times respectively, each extraction time is 1-2 hour, go medicinal residues to merge three medicinal liquids, filter, cross the polyamide column adsorption column, the medicinal liquid of holding back after the absorption of polyamide column adsorption column is crossed macroporous adsorptive resins, use the triplication water washing, the alcohol desorption of reuse 60-90%, eluent concentrates, and uses ethyl acetate extraction three times, collect the ethyl acetate part, concentrate drying gets Ginkgo total lactones;
Total lactone is mixed sample with silica gel 1-2 weight portion, and last silicagel column separates, and uses the chloroform-methanol gradient elution, gets bilobalide and ginkgolectone AB;
Ginkgolectone AB gets ginkalide B through recrystallization repeatedly.
5, a kind of as claim 1,2,3 or 4 described methods, it is characterized in that the high ratio with diameter of post of polyamide column, macroporous adsorptive resins or three kinds of adsorption columns of silicagel column in this method is 4-15; Concentration of alcohol is 70%.
6, ask the method for 1,2,3 or 4 described extraction Folium Ginkgo extract according to right, it is characterized in that antioxidant in this method is 0.5% vitamin C, sodium sulfite or sodium pyrosulfite.
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| CNB011198249A CN1173724C (en) | 2001-06-29 | 2001-06-29 | Systemic separation process and prepn of ginkgetin, ginkgolide and bilobalide |
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| CNB011198249A CN1173724C (en) | 2001-06-29 | 2001-06-29 | Systemic separation process and prepn of ginkgetin, ginkgolide and bilobalide |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100408033C (en) * | 2005-09-29 | 2008-08-06 | 刘晓东 | Fat emulsion of biobalide B and preparation method |
| CN102000125B (en) * | 2010-11-17 | 2013-11-06 | 江振鸣 | Ginkgo flavone extraction method |
| CN102416027B (en) * | 2011-12-01 | 2015-11-25 | 徐州医学院 | The application of active substance in treatment cardiovascular and cerebrovascular diseases medicament of Semen Ginkgo active component extraction separating method and extraction |
| CN102526025A (en) * | 2011-12-31 | 2012-07-04 | 浙江康恩贝制药股份有限公司 | Method for preparing ginkgo leaf extractive containing a plurality of appointed active ingredients |
| CN105372338A (en) * | 2014-08-08 | 2016-03-02 | 南京中科药业有限公司 | Compound yinlingtong capsule quality detection method |
| CN105456309A (en) * | 2015-12-17 | 2016-04-06 | 东北林业大学 | Process for purifying ginkgetin in gingko extract through anti-solvent recrystallization method |
| CN106491665A (en) * | 2016-09-26 | 2017-03-15 | 合肥信达膜科技有限公司 | A kind of GINKGO BILOBA EXTRACT film separation system and method |
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Assignee: Sichuan Kechuang Medicine Group Co., Ltd. Assignor: Xinshiji Science and Technology Co., Ltd., Chengdu Contract record no.: 2010510000020 Denomination of invention: Systemic separation process and prepn of ginkgetin, ginkgolide and bilobalide Granted publication date: 20041103 License type: Exclusive License Open date: 20020213 Record date: 20100512 |
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Granted publication date: 20041103 Termination date: 20160629 |