CN101780122B - Preparation method of a water-soluble gingko extract - Google Patents
Preparation method of a water-soluble gingko extract Download PDFInfo
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- CN101780122B CN101780122B CN2010101170942A CN201010117094A CN101780122B CN 101780122 B CN101780122 B CN 101780122B CN 2010101170942 A CN2010101170942 A CN 2010101170942A CN 201010117094 A CN201010117094 A CN 201010117094A CN 101780122 B CN101780122 B CN 101780122B
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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 method for preparing of Semen Ginkgo extrac.
Background technology
Folium Ginkgo is claimed 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 method for distilling 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 generally acknowledging in the world is flavones ingredient >=24%, and lactone >=6% (the Semen Ginkgo extrac progress. China brewages, and 2009,1:14-18), orally-ingestible is used with injection, is widely used in multiple diseases such as cardiovascular and cerebrovascular disease.The GBE that supplies injection to use 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.Through retrieval; Domesticly existing surpass 70 patent applications that relate to Folium Ginkgo extract, for example CN02134490.6 number " a kind of method for preparing of Folium Ginkgo extract ", CN02129905.6 number " a kind of high-activity ginkgo leaf extract preparation and purposes ", CN03114825.5 number " method for preparing of Folium Ginkgo extract ", CN03114826.3 number " method for preparing of extractive of low acidic gingko leaves ", CN200410069037.6 number " a kind of Folium Ginkgo extract and method for distilling thereof " etc.These applications all belong to the method for from Folium Ginkgo, extracting general GBE.
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 bullion 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, takes this technology to be difficult to guarantee the content of lactone and the water solublity of finished product simultaneously, and 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 ", and this technology is extracted for adopting to stir when bullion prepares water solubility extract, leaves standstill; Filter, add aqueous gelatin solution and precipitate, leave standstill again; Filter, vacuum concentration adds anhydrous alcohol solution again to doing; 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 CE 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, filtrating 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.Like 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, provide the rate of transform of a kind of soluble flavone and total lactone high, raw material availability is high, but the method for preparing of the water-soluble gingko extract of the low injection of production cost.
A kind of method for preparing 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 after concentrating filter liquor, the drying, and solid is used C
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 method for preparing of above-mentioned water-soluble gingko extract; Said 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 items).
In the method for preparing 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 method for preparing of above-mentioned water-soluble gingko extract, C described in the step (1)
2-C
8Alkane is preferably petroleum ether or gasoline.
In the method for preparing 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 method for preparing 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 method for preparing of above-mentioned water-soluble gingko extract, the acid amide type resin is preferably ADS-F8 described in the step (3).
In the method for preparing 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 said middle concentration alcoholic solution is 50～70% alcoholic solution.
In the method for preparing 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 method for preparing of above-mentioned water-soluble gingko extract, alcoholic solution is preferably methanol solution or alcoholic solution described in step (3) or (4).
In the method for preparing 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 method for preparing 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 rate of transform of soluble flavone that method for preparing of the present invention obtains and total lactone high, raw material availability is high, can reduce production costs.
Further set forth technical scheme of the present invention through specific embodiment below.
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, filtration, 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, use the water elution remove impurity; 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, extraction 60min, 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, and discharging behind the extraction 60min is filtered; 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; 70% ethanol elution is used in the back; 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 (6)
1. the method for preparing 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 after concentrating filter liquor, the drying, and solid is used C
2-C
8Alkane desilverization Fructus Pruni phenolic acid gets the Ginkgo total lactones of dephenolize acid;
Said Semen Ginkgo extrac is commercially available Semen Ginkgo extrac, and its flavones content is 22.0-26.0%, and lactone content is 4.0-7.0%;
(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; Said acid amide type resin is a polyamide;
Said low concentration alcoholic solution accounts for cumulative volume than the solution that is 0～30% for alcohol, and said intermediate concentration alcoholic solution is 50～70% alcoholic solution;
(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; Said deacidification Ginkgo total lactones is earlier with the dissolving of 20～100% alcoholic solutions, again with intermediate concentration alcohol eluen partially mixed after concentrated; Said drying is a spray drying.
2. the method for preparing 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 method for preparing of water-soluble gingko extract according to claim 1 is characterized in that in the step (1) said C
2-C
8Alkane is petroleum ether or gasoline.
4. the method for preparing of water-soluble gingko extract according to claim 1 is characterized in that in the step (1) said solid and C
2-C
8The w/v of alkane is 1: 4～1: 20.
5. the method for preparing 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 method for preparing of water-soluble gingko extract according to claim 1 is characterized in that in step (3) or (4), said alcoholic solution is methanol solution or alcoholic solution.
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| 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 |
Citations (2)
| 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 |
| CN101199560A (en) * | 2007-12-27 | 2008-06-18 | 扬子江药业集团有限公司 | Ginkgo leaf extract and preparing method thereof |
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Patent Citations (2)
| 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 |
| CN101199560A (en) * | 2007-12-27 | 2008-06-18 | 扬子江药业集团有限公司 | Ginkgo leaf extract and preparing method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 卢起来等.银杏叶中有效成分的提取.《武汉化工学院学报》.1999,第21卷(第3期),第20-22页. * |
| 杨爱萍等.银杏叶中黄酮提取工艺的改进.《莱阳农学院学报》.2001,第18卷(第3期),第191-192页. * |
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