CN101780122A - Preparation method of a water-soluble gingko extract - Google Patents
Preparation method of a water-soluble gingko extract Download PDFInfo
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Abstract
The invention discloses a preparation method of a water-soluble gingko extract, comprising the following steps: taking the gingko extract as material and ethyl acetate as a solvent for extraction, filtering, concentrating and drying the filtrate to obtain solid which remove ginkgolic acid with C2-C8 alkane, and obtaining total terpene lactone with removing of phenolic acid; (2) adding water to extract substances which are not dissolved in the ethyl acetate, filtering or centrifuging and obtaining upper column clear liquid; (3) for amide-type resin columns on the clear liquid, firstly using low-concentration alcohol solution to elute and remove impurities, then using medium-concentration alcohol to elute, collecting the eluent of the medium-concentration alcohol solution, concentrating and then obtaining concentrated water-soluble flavone part; (4) using an alcohol solution to dissolve the total terpene lactones with removing of phenolic acid, mixing evenly with the concentrated water-soluble flavone part, drying and obtaining the water-soluble gingko extract, wherein the content of flavone is 24-45 percent, the content of lactone is 6-12 percent, the water solubility is more than or equal to 5 perecnt, the ginkgolic acid is less than or equal to 1ppm, the water-soluble gingko extract does not contain protein and tannin and can be used for injection. The obtained soluble flavone and the total terpene lactone has high transferring rate, the utilization ratio of the materials is high, and the production cost can be reduced.
Description
Technical field
The present invention relates to the preparation method of Semen Ginkgo extrac.
Background technology
Folium Ginkgo claims Folium Ginkgo again, is the leaf of Ginkgoaceae plant Ginkgo biloba (Ginkgo biloba L.), and its bitter and puckery flavor, property are flat, and because of it contains flavonoid glycoside and the terpene lactones composition is used as medicine, the useful heart is astringed the lung, removing dampness antidiarrheal effect.In recent years, people constantly study the medical value and the extracting method of Folium Ginkgo, and are wherein more successful with Folium Ginkgo extract (being called for short GBE) application, use extensively.
Semen Ginkgo extrac is to be raw material with the Semen Ginkgo, adopts a series products of appropriate solvent effective component extracting.The content standard of the ginkgo agent of Gong Rening is flavones ingredient 〉=24% in the world, and lactone 〉=6% (the Semen Ginkgo extrac progress. China brewages, and 2009,1:14-18), can orally use with injection, be widely used in multiple diseases such as cardiovascular and cerebrovascular disease.The GBE that uses for injection has higher requirements to water solublity, protein, tannin, and biological activity and safety in utilization can be more secure, are one of present Semen Ginkgo extrac developing direction.
The method of extracting Folium Ginkgo GBE at present is a lot of, and many processes have all been applied for patent of invention.By retrieval, domesticly existing surpass 70 patent applications that relate to Folium Ginkgo extract, for example CN02134490.6 number " a kind of preparation method of Folium Ginkgo extract ", CN02129905.6 number " a kind of high-activity ginkgo leaf extract preparation and purposes ", CN03114825.5 number " preparation method of Folium Ginkgo extract ", CN03114826.3 number " preparation method of extractive of low acidic gingko leaves ", CN200410069037.6 number " a kind of Folium Ginkgo extract and extracting method thereof " etc.These applications all belong to the method for extracting general GBE from Folium Ginkgo.
Extract the 3 pieces of patents that have of water soluble ginkgo leaf extract: application number is that 02113533.9 patent has been introduced a kind of " production technology of water soluble ginkgo leaf extract ", this technology is the conventional macroporous resin adsorption resin of employing when crude product prepares water solubility extract, because resin is to the adsorptivity of flavone and lactone, the difference of lactone and flavonoid glycoside water-soluble etc. is all very big, take this technology to be difficult to guarantee the content of lactone and the water solublity of finished product simultaneously, loss of effective components is bigger.
Application number is that CN200510003243.1 has reported " a kind of production method of water soluble ginkgo leaf extract ", this technology is extracted for adopting to stir when crude product prepares water solubility extract, leaves standstill, and filters, adding aqueous gelatin solution precipitates, leave standstill, filter, vacuum concentration is to doing, add anhydrous alcohol solution again, filter, vacuum concentration is also dry, and the mode of pulverizing prepares water solublity GBE.Because lactone to water and methanol, the insoluble or indissoluble of alcoholic acid weak solution, adds the precipitation of gelatin, effective ingredient, especially the lactone loss is bigger.Also, can't adopt this technology controlling and process to obtain content specification and controlled relatively finished product because the difference of leaf source, quality and the processing technique of crude extract causes component difference very big.
Application number is the patent of 200810060422.2 " a kind of production technologies of water soluble ginkgo leaf extract ", with the Semen Ginkgo leaf is raw material, common process makes it fully dissolve back recovery ethanol to thick paste with ethanol after getting extract, add an amount of ethanol again, extract 2～4 times after-filtration, filtrate is concentrated into thick paste; With purified water extraction 2～4 times, the extracting solution cold filtration concentrates, and is drying to obtain water soluble ginkgo leaf extract with thick paste.In this technology because of need extract and concentration process through heating for multiple times, the easy oxidation of flavone and losing, filter process repeatedly also causes the loss of total lactone composition easily, content of tannin is higher.
Also have at home and earlier use the ethyl acetate extraction Ginkgo total lactones, dissolve insoluble part with alkaline water then, solution superamide type resin prepares exquisite flavone part, is mixed then to not requiring water miscible Semen Ginkgo extrac bibliographical information.As patent application CN200710191922.5 " a kind of Folium Ginkgo extract and preparation method thereof ", be raw material also with commercially available Semen Ginkgo extrac, carry lactone through petroleum ether deacidification, ethyl acetate.Ethyl acetate extract passes through acetone solution again, and refinement treatment such as peroxidating aluminum get exquisite lactone.And be insoluble to the solid of ethyl acetate, with the sodium carbonate liquor dissolving, cross the AB-8 post, cross polyamide column then, purified flavone.Two parts are mixed into Semen Ginkgo extrac again.This scheme is owing to adopt the aqueous sodium carbonate dissolving to be insoluble to the ethyl acetate thing, obtain after being mixed be water (pH=7) water solublity relatively poor relatively be used for oral Semen Ginkgo extrac.This process goal be for can measure the high extract of content, and do not require water solublity, and its technology is also more complicated, in addition, the acid stripping method that this scheme adopts is that extract is directly used petroleum ether extraction, and flavones ingredient is heated and oxidation easily, and the effective ingredient rate of transform is descended.Therefore, technology all can not satisfy the requirement of Semen Ginkgo extrac deep processing upgraded product to raw material fully at present.
Summary of the invention
The objective of the invention is to overcome the deficiency that prior art exists, the rate of transform height of a kind of soluble flavone and total lactone is provided, raw material availability height, but the preparation method of the water-soluble gingko extract of the low injection of production cost.
A kind of preparation method of water-soluble gingko extract comprises the steps:
(1) being raw material with the Semen Ginkgo extrac, is solvent extraction with the ethyl acetate, filters, and gets solid, solid C after concentrating filter liquor, the drying
2-C
8Alkane desilverization Fructus Pruni phenolic acid gets dephenolize acid Ginkgo total lactones;
(2) insoluble matter of above-mentioned ethyl acetate extraction adds water stirring extraction, and filtration or centrifugal obtains upper column clear liquid;
(3) acid amide type resin column on the clear liquid, earlier with the remove impurity of low concentration alcoholic solution eluting, reuse intermediate concentration alcoholic solution eluting, the eluent of collection intermediate concentration alcoholic solution obtains concentrating the water-soluble flavone part after concentrating;
(4) dephenolize acid Ginkgo total lactones dissolves with alcoholic solution, and is partially mixed with the water-soluble flavone after concentrating, the dry water-soluble gingko extract that gets.
In the preparation method of above-mentioned water-soluble gingko extract, described Semen Ginkgo extrac is commercially available Semen Ginkgo extrac, its flavones content is 22.0-26.0%, and lactone content is 4.0-7.0% (flavone, lactone and total phenolic content assay method are seen 2005 editions＜Chinese Pharmacopoeia〉Semen Ginkgo extrac relevant item).
In the preparation method of above-mentioned water-soluble gingko extract, in the step (1) be that the time of solvent extraction is preferably 0.5 ~ 5 hour with the ethyl acetate.
In the preparation method of above-mentioned water-soluble gingko extract, C described in the step (1)
2-C
8Alkane is preferably petroleum ether or gasoline.
In the preparation method of above-mentioned water-soluble gingko extract, solid and C described in the step (1)
2-C
8The w/v of alkane is preferably 1: 4 ~ and 1: 20.
In the preparation method of above-mentioned water-soluble gingko extract, the water that the insoluble matter of ethyl acetate extraction adds 4 ~ 20 times of volumes in the step (2) stirs discharging behind 30 ~ 120min.
In the preparation method of above-mentioned water-soluble gingko extract, the acid amide type resin is preferably ADS-F8 described in the step (3).
In the preparation method of above-mentioned water-soluble gingko extract, low concentration alcoholic solution described in the step (3) accounts for cumulative volume than 0～30% alcoholic solution for alcohol, and described middle concentration alcoholic solution is 50～70% alcoholic solution.
In the preparation method of above-mentioned water-soluble gingko extract, dephenolize described in the step (4) acid Ginkgo total lactones is earlier with the dissolving of 20～100% alcoholic solutions, again partially mixed after concentrated with the intermediate concentration alcohol eluen.
In the preparation method of above-mentioned water-soluble gingko extract, alcoholic solution is preferably methanol solution or alcoholic solution described in step (3) or (4).
In the preparation method of above-mentioned water-soluble gingko extract, drying is preferably spray drying, vacuum drying or lyophilization described in the step (4).
Compared with prior art, the present invention has following beneficial effect:
1. the water-soluble gingko extract that utilizes preparation method of the present invention to obtain, its flavones content are that 24-45% and lactone content are 6-12%, water-soluble degree 〉=5%, and gingkolic acid≤1ppm does not contain protein and tannin, but injection.
2. utilize the soluble flavone that preparation method of the present invention obtains and the rate of transform height of total lactone, the raw material availability height can reduce production costs.
Further set forth technical scheme of the present invention below by specific embodiment.
The specific embodiment
The flavones content of the commercially available Semen Ginkgo extrac that following examples are used is 22.0-26.0%, and lactone content is 4.0-7.0% (flavone, lactone and total phenolic content assay method are seen＜Chinese Pharmacopoeia〉Semen Ginkgo extrac relevant item).
Following alcoholic acid percentage ratio is percent by volume.
Embodiment 1
Semen Ginkgo extrac 30kg adds the 150L ethyl acetate, and stir speed (S.S.) 60rm/min extracts 60min, filters, and the recovery ethyl acetate refluxes with the 150L petroleum ether after extremely doing, and discards petroleum ether, gets the total lactone of desilverization Fructus Pruni phenolic acid.Be insoluble to the ethyl acetate solid and add 240L water, under stir speed (S.S.) 60rm/min, discharging behind the extraction 60min, behind the medicinal liquid high speed centrifugation, cross the ADS-F8 resin, wash with water remove assorted, use 60% ethanol elution then, collect the 60 ℃ of concentrating under reduced pressure in 60% ethanol position, after being mixed with Ginkgo total lactones dissolve with ethanol liquid, spray drying obtains water-soluble gingko extract.Measure according to official method, flavones content is 27.2%, and lactone content is 6.5, water solubility 〉=5%, and ginkgoic acid content＜1ppm does not contain albumen and tannin.
Embodiment 2
Semen Ginkgo extrac 30Kg adds the 300L ethyl acetate, under stir speed (S.S.) 100rm/min, extracts 30min, filters, and the recovery ethyl acetate refluxes with the 180L normal hexane after extremely doing, and discards normal hexane, must take off the total lactone of ginkgoic acid.The solid that is insoluble to ethyl acetate adds water 280L under stir speed (S.S.) 100rm/min, discharging behind the extraction 60min, high speed centrifugation, medicinal liquid is crossed polyamide, with 5% ethanol elution remove impurity, use 60% ethanol elution then, collect the 60 ℃ of concentrating under reduced pressure in 60% ethanol position, after being mixed with the dissolve with ethanol liquid of the total lactone of deacidification, 60 ℃ of following drying under reduced pressure are to water-soluble gingko extract.Measure according to official method, flavones content is 29.2%, and lactone content is 7.8%, water solubility 〉=5%, and ginkgoic acid content＜1ppm does not contain albumen and tannin.
Embodiment 3
Semen Ginkgo extrac powder 30g, adding while stirring has the 200ml ethyl acetate, under stir speed (S.S.) 120rm/min, extracts 60min, and the recovery ethyl acetate refluxes with 210mL gasoline after extremely doing, and discards gasoline, gets the total lactone of deacidification.The solid that is insoluble to ethyl acetate adds deionization 240mL water under stir speed (S.S.) 120rm/min, discharging behind the extraction 60min, filter, medicinal liquid is crossed the ADS-F8 resin, with 10% ethanol remove impurity, use 50% ethanol elution then, collect the 60 ℃ of concentrating under reduced pressure in 50% ethanol position, after being mixed with the dissolve with ethanol liquid of the total lactone of deacidification, spray drying obtains water-soluble gingko extract.Measure according to official method, its flavones content is 28.2%, and lactone content is 6.4%, water solubility 〉=5%, and ginkgoic acid content＜1ppm does not contain albumen and tannin.
Embodiment 4
Shown in embodiment 1, different is: medicinal liquid is crossed the ADS-F8 resin, with 15% ethanol elution remove impurity, back 70% ethanol elution, collect the 60 ℃ of concentrating under reduced pressure in 70% ethanol position, after being mixed with the dissolve with ethanol liquid of the total lactone of deacidification, lyophilization obtains water-soluble gingko extract.Measure according to official method, its flavones content is 32.2%, and lactone content is 8.4%, water solubility 〉=5%, and ginkgoic acid content＜1PPm does not contain albumen and tannin.
Embodiment 5
Shown in embodiment 2, different is: medicinal liquid is crossed polyamide, adopts 20% ethanol elution remove impurity, reuse 60% ethanol elution, collect the 60 ℃ of concentrating under reduced pressure in 60% ethanol position, after being mixed with the dissolve with ethanol liquid of the total lactone of deacidification, 60 ℃ of vacuum dryings obtain water-soluble gingko extract.Measure according to official method, its flavones content is 39.7%, and lactone content is 10.4, water solubility 〉=5%, and ginkgoic acid content＜1ppm does not contain albumen and tannin.
Embodiment 6
Shown in embodiment 3, different is: medicinal liquid is crossed the ADS-F8 resin, with 30% ethanol elution remove impurity, use 60% ethanol elution then, collect the 60 ℃ of concentrating under reduced pressure in 60% ethanol position, after being mixed with the dissolve with ethanol liquid of the total lactone of deacidification, lyophilization obtains water-soluble gingko extract.Measure according to official method, its flavones content is 44.2%, and lactone content is 11.9%, water solubility 〉=5%, and ginkgoic acid content＜1ppm does not contain albumen and tannin.
Claims (10)
1. the preparation method of a water-soluble gingko extract is characterized in that comprising the steps:
(1) being raw material with the Semen Ginkgo extrac, is solvent extraction with the ethyl acetate, filters, and gets solid, solid C after concentrating filter liquor, the drying
2-C
8Alkane desilverization Fructus Pruni phenolic acid gets the Ginkgo total lactones of dephenolize acid;
(2) insoluble matter of above-mentioned ethyl acetate extraction adds water stirring extraction, and filtration or centrifugal gets upper column clear liquid;
(3) acid amide type resin column on the clear liquid, earlier with the remove impurity of low concentration alcoholic solution eluting, reuse intermediate concentration alcoholic solution eluting, the eluent of collection intermediate concentration alcoholic solution obtains concentrating the water-soluble flavone part after concentrating;
(4) the deacidification Ginkgo total lactones dissolves with alcoholic solution, and is partially mixed evenly with concentrated water-soluble flavone, the dry water-soluble gingko extract that gets.
2. the preparation method of water-soluble gingko extract according to claim 1 is characterized in that in the step (1), is that the time of solvent extraction is 0.5 ~ 5 hour with the ethyl acetate.
3. the preparation method of water-soluble gingko extract according to claim 1 is characterized in that in the step (1) described C
2-C
8Alkane is petroleum ether or gasoline.
4. the preparation method of water-soluble gingko extract according to claim 1 is characterized in that in the step (1) described solid and C
2-C
8The w/v of alkane is 1: 4 ~ 1: 20.
5. the preparation method of water-soluble gingko extract according to claim 1 is characterized in that in the step (2), and the water that the insoluble matter of ethyl acetate extraction adds 4 ~ 20 times of volumes stirs discharging behind 30 ~ 120min.
6. the preparation method of water-soluble gingko extract according to claim 1 is characterized in that in the step (3), described acid amide type resin is ADS-F8 or polyamide.
7. the preparation method of water-soluble gingko extract according to claim 1 is characterized in that in the step (3), described low concentration alcoholic solution be alcohol to account for the cumulative volume ratio be 0 ~ 30% solution, described intermediate concentration alcoholic solution is 50 ~ 70% alcoholic solution.
8. the preparation method of water-soluble gingko extract according to claim 1 is characterized in that in the step (4), and described deacidification Ginkgo total lactones is earlier with the dissolving of 20 ~ 100% alcoholic solutions, again with intermediate concentration alcohol eluen partially mixed after concentrated.
9. according to the preparation method of claim 1 or 8 described water-soluble gingko extracts, it is characterized in that in step (3) or (4), described alcoholic solution is methanol solution or alcoholic solution.
10. the preparation method of water-soluble gingko extract according to claim 1 is characterized in that the described drying of step (4) is spray drying, vacuum drying or lyophilization.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102416027A (en) * | 2011-12-01 | 2012-04-18 | 徐州医学院 | Gingkgo active ingredient extraction and separation method and use of extracted active matters in medicines for treating cardiovascular and cerebrovascular diseases |
| CN106109510A (en) * | 2016-01-27 | 2016-11-16 | 河北润茂制药有限公司 | Fine silver flavone extraction process |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1362252A (en) * | 2001-12-31 | 2002-08-07 | 黄名华 | Method of eliminating gingkolic acid from gingko extract |
| CN101199560B (en) * | 2007-12-27 | 2012-04-25 | 扬子江药业集团有限公司 | Ginkgo leaf extract and preparing method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102416027A (en) * | 2011-12-01 | 2012-04-18 | 徐州医学院 | Gingkgo active ingredient extraction and separation method and use of extracted active matters in medicines for treating cardiovascular and cerebrovascular diseases |
| 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 |
| CN106109510A (en) * | 2016-01-27 | 2016-11-16 | 河北润茂制药有限公司 | Fine silver flavone extraction process |
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Owner name: GUANGZHOU HANFANG PHARMACEUTICAL CO., LTD. Free format text: FORMER NAME: HANFANG MODEM CHINESE TRADITIONAL MEDICINE RESEARCH DEVELOPMENT CO., LTD., GUANG |
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