CN102603482A - Separation technology for multiple components in ginkgo leaf - Google Patents
Separation technology for multiple components in ginkgo leaf Download PDFInfo
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- 241000218628 Ginkgo Species 0.000 title claims abstract description 57
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- 238000000926 separation method Methods 0.000 title claims abstract description 23
- 238000005516 engineering process Methods 0.000 title description 3
- 238000000605 extraction Methods 0.000 claims abstract description 52
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- 238000003756 stirring Methods 0.000 claims description 9
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- YXHVCZZLWZYHSA-FPLPWBNLSA-N Ginkgoic acid Chemical class CCCCCC\C=C/CCCCCCCC1=CC=CC(O)=C1C(O)=O YXHVCZZLWZYHSA-FPLPWBNLSA-N 0.000 claims description 3
- 239000004695 Polyether sulfone Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
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- BDMCAOBQLHJGBE-UHFFFAOYSA-N C60-polyprenol Natural products CC(=CCCC(=CCCC(=CCCC(=CCCC(=C/CCC(=C/CCC(=C/CCC(=C/CCC(=C/CCC(=C/CCC(=C/CCC(=C/CO)C)C)C)C)C)C)C)C)C)C)C)C BDMCAOBQLHJGBE-UHFFFAOYSA-N 0.000 abstract 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention discloses a separation technique for multiple components in ginkgo leaves. Ginkgo leaves are used as a raw material. By combination of ultrasonic extraction and supercritical CO2 extraction-distillation, separation of multiple effective components is realized. The separation technique provided by the invention comprises the following steps: firstly, extracting the ginkgo leaves by ultrasonication in ethanol solutions with different concentrations for two times, and carrying out the following processes on filter liquor and filter residue obtained by filtration: (1) carrying out supercritical CO2 extraction and separation on the filter residue to obtain polyprenol compounds, and separating raffinate by water extraction and alcohol precipitation to obtain ginkgo polysaccharides; and (2) carrying out ultrafiltration and concentration on the filter liquor, and firstly separating to obtain ginkgolic acids by the supercritical CO2 extraction at a proper temperature and a proper pressure; and changing extraction conditions, starting a rectifying column, heating by the temperature variation in the axial direction in four segments, and continuously extracting and separating to obtain ginkgo terpene lactones and flavonoid compounds. The separation technique provided by the invention has the advantages that active ingredients are difficult to decompose or destroy, harmful chemical reagent residues do not exist, the extraction efficiency is high, the separation effect is good and the like, solves the problem that the content of poisonous phenolic acid in ginkgo leaf extract exceeds the standard, and is an environment-friendly, economic and industrialization-suitable technique.
Description
Technical field
The invention belongs to the herbal component separation field, be specifically related to the multi-component stripping technique of a kind of Ginkgo Leaf.
Background technology
Ginkgo Leaf has very high pharmaceutical use, in China's successive dynasties traditional Chinese medical science treatise, all previous pharmacopeia and external numerous research, has all put down in writing Ginkgo Leaf and medicinal efficacy thereof.Research shows that it is its important factor with extensive pharmacological action that Ginkgo Leaf contains the particular chemical composition.Up to now, the compound of in Ginkgo Leaf, finding has reached kind more than 160, comprising: compositions such as flavonoid, terpene lactone, polyose, phenolic acids, polypenthylene alcohols.
The domestic and international at present separation to active skull cap components in the Ginkgo Leaf, further investigation utilization mainly concentrate on aspects such as flavonoid and terpene lactone, and fewer to the research and utilization of phenolic acids, polypenthylene alcohols, polyose.And tradition thinks that separating Ginkgo phenolic acids has cytotoxicity, can cause allergy, mutagenesis, can cause clonic spasm, neural paralysis, therefore is taken as objectionable impurities by strictness restriction and removal at the ginkgo goods; The polypenthylene alcohols is used as a kind of useless composition and is removed in most of Folium Ginkgo extract productions, seldom these two types of materials of enrichment.Discovered in recent years; The total amount of separating Ginkgo phenolic acids account for the ginkgo cured leaf heavy 1.0%~2.0%; Belong to the higher material of content, have intensive desinsection, restraining and sterilizing bacteria effect and antitumor, anti-inflammatory and multiple pharmacologically active such as anti-oxidant, can be used for the exploitation of plant pesticide and the research of new drug; Polypenthylene alcohols content is 1.0%~2.0%; Being higher than ginkgolic flavone glycoside and terpene lactone, is 100 times of human body dolichol content, has tangible biological activity; Have antitumor, auxiliary chemoradiotherapy, promote apoptosis of tumor cells, antiviral and protection liver injury and immunoregulatory pharmacological action; Polysaccharides from ginkgo biloba has immunomodulatory, antitumor, the anti-ageing various active effect of waiting for a long time.
Ginkgo Leaf component stripping technique is not seen the report that has separation simultaneously to obtain ginkgolic flavone glycoside class, terpene lactone, polypenthylene alcohols, polysaccharides from ginkgo biloba and phenolic acids at present.There is following weak point in existing method: one, the long-time high temperature extraction of water or organic solvent can decompose components such as destroying flavonoid, terpene lactone; Two, use poisonous and harmful solvents such as acetone beyond the ethanol, methyl alcohol, chloroform, sherwood oil, ETHYLE ACETATE, caused the product hazardous solvent residual, can't be used for suitability for industrialized production; Three, the toxic substance separating Ginkgo phenolic acids in the Ginkgo Leaf is not effectively controlled, and most of product can't reach the NF requirement; Four, utilize solvent method to extract, shortcoming such as the method for carrying out separation and purification with column chromatography or HPLC then exists extraction time long, and efficient is low, and solvent load is big.
Summary of the invention
The object of the present invention is to provide the multi-component stripping technique of a kind of Ginkgo Leaf, adopt ultrasonic method to extract the compound effective constituent of Ginkgo Leaf earlier, and then leave each component through technical points such as ultrafiltration, supercritical extraction, rectifying.The present invention have effective constituent be difficult for being decomposed destruction, do not have advantages such as harmful chemical agent residue, extraction efficiency height, good separating effect; Solved the problem that the poisonous phenolic acid of Folium Ginkgo extract exceeds standard simultaneously, but be the technology of not only environmental protection, economy but also an industrializing implementation.
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
Ginkgo Leaf polycomponent stripping technique step of the present invention is following:
(1) get qualified Ginkgo Leaf and carry out pre-treatment: removal of impurities also is dried to moisture≤5%, pulverizes the 10-24 mesh sieve.
(2) add 75-90% alcohol dipping 60-90 minute that 10-12 doubly measures in the raw material, at power 3000-4000W, supersound extraction 30-40min after-filtration under temperature 40-45 ℃ the condition; The ethanol ultrasonic extraction of the 60-75% that filter residue is doubly measured with 10-12 again, condition is the same, filters, and merges filtrate for later use twice.
(3) step (2) filter residue is adopted supercritical CO
2Extraction, condition is: extraction kettle pressure 25-30MPa, extraction temperature 50-55 ℃; 40 ℃ of separation temperatures, I level separating still pressure 8-10MPa, II level separating still pressure 6MPa, CO
2Flow velocity 2-2.5L/min (food grade, purity>=99.5%), the extraction 4-5h, separating still collect polypenthylene alcohols oily matter, extract remainder is subsequent use.
(4) in step (3) extract remainder, add 8-10 times of water gaging, 100 ℃ decoct 2h, filter and collect the water extract; The water extract is concentrated into the 1/8-1/l0 of original volume; Add the absolute ethyl alcohol of 5 times of amounts after the cooling, stir, 1-4 ℃ of airtight refrigeration 12h; Centrifugal 8-10min under the 3000-4000r/min condition then, separate throw out; In throw out, add 5 times of amount 80% ethanol again, stir, the centrifugal 8-10min of 3000-4000r/min precipitates the dry polysaccharides from ginkgo biloba that gets.
The ultra-fine filter that the filtrating of (5) step (2) being collected is passed through molecular weight cut-off 10000D adopts the sulfonated polyether sulfone flat plate ultrafiltration membrane, and the control ultrafiltration pressure is 0.20~0.25MPa; Temperature is 25-30 ℃ and carries out ultrafiltration repeatedly; When the trapped fluid volume reduces to 1/l0, add 75% ethanol of 5 times of volumes, continue ultrafiltration; When the trapped fluid volume be reduced to once more original volume 1/10 the time; Stop ultrafiltration, collect the ultrafiltration filtered solution, 45-50 ℃ of vacuum decompression is concentrated into the liquid concentrator volume: Ginkgo Leaf crude drug=1: 1 (ml: g).(6) liquid concentrator is adopted supercritical CO
2The equipment extraction, condition is: extraction kettle pressure 10-16MPa, extraction temperature 35-40 ℃; 35 ℃ of separation temperatures, I level separating still pressure 8-10MPa, II level separating still pressure 6MPa, CO
2Flow velocity 1.5-2L/min (food grade, purity>=99.5%), extraction 30-45 min collects extract and gets the separating Ginkgo phenolic acids alcohol mixeding liquid.The water that adds 5 times of volumes in the extract stirs 1-4 ℃ of airtight refrigeration 12h; Centrifugal 8-10min under the 3000-4000r/min condition then, collecting precipitation gets the ginkgolic acid compounds.
(7) extraction conditions is adjusted into: extraction kettle pressure 20-28MPa, extraction temperature 45-50 ℃, launch rectifying volumn (dividing four-section ladder degree temperature control), setting is followed successively by from the temperature to capital at the bottom of the post: 45 ℃, 50 ℃, 55 ℃, 60 ℃; 40 ℃ of separation temperatures; Separating still pressure 5-8MPa; Continue extraction 50-70 min, collect extract at times, get ginkgo terpene lactone, flavonoid ethanolic soln respectively; Being concentrated into specific density in 45-50 ℃ of vacuum decompression is 1.10-1.20 (40 ℃), and the liquid concentrator vacuum lyophilization gets ginkgo terpene lactone, flavonoid compound respectively.
Filtering among the present invention and all adopting the order number is 200-300 purpose screen cloth; Concentration of ethanol is volume percent.
Owing to receive the influence in the age of tree and picking season; Active constituent content in the Ginkgo Leaf changes greatly; Almost can not be according to the big Ginkgo Leaf of the bibliographical information age of tree as the raw material of producing Folium Ginkgo extract, so the used raw material of the present invention is preferably the 2-3 age of tree, the Ginkgo Leaf in 5-9 month.
It is preferred 85% to extract for the first time the alcohol concn of usefulness in the above-mentioned steps (2), extracts the alcohol concn preferred 70% of usefulness for the second time.
Extraction conditions is preferred in the above-mentioned steps (6): extraction kettle pressure 14MPa, 38 ℃ of extraction temperature; 35 ℃ of separation temperatures, I level separating still pressure 9MPa, II level separating still pressure 6MPa, CO
2Flow velocity 1.8L/min (food grade, purity>=99.5%) extracts 45 min.
Remarkable advantage of the present invention is: 1) effectively overcome and destroyed composition, poisonous chemical agent residue in the prior art, be unfavorable for shortcomings such as suitability for industrialized production; 2) separation obtains ginkgolic flavone glycoside class, terpene lactone, polypenthylene alcohols, separating Ginkgo phenolic acids, polysaccharides from ginkgo biloba simultaneously, good separating effect, target components purity height; 3) solved the problem that the poisonous phenolic acid of Folium Ginkgo extract exceeds standard.The above-mentioned all kinds of materials of enrichment can be applied to it research and development of industries such as protective foods, makeup, new drug and plant pesticide as raw material, midbody.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Following embodiment can help those skilled in the art more fully to understand the present invention, but does not limit the present invention in any way.
Embodiment 1: the Ginkgo Leaf component is separated
Raw material: the Ginkgo Leaf that pluck the 3 years age of tree, June.
Step:
(1) with the Ginkgo Leaf removal of impurities, be dried to moisture≤5%, pulverize weighing 10-24 purpose Ginkgo Leaf 3000g.
(2) add 85% alcohol dipping 60 minutes of 10 times of amounts,, extract the 30min after-filtration under 42 ℃ the condition at ultrasonic power 2800W; Filter residue is used 70% ethanol ultrasonic extraction of 10 times of amounts again, and condition is the same, filters, and merges filtrate for later use twice.
(3) step (2) filter residue is carried out supercritical CO
2Extraction, condition is: extraction kettle pressure 26MPa, 52 ℃ of extraction temperature; 40 ℃ of separation temperatures, I level separating still pressure 9MPa, II level separating still pressure 6MPa, CO
2Flow velocity 2.2L/min (food grade, purity>=99.5%), the extraction 4h, separating still collect polypenthylene alcohols oily matter, extract remainder is subsequent use.
(4) in step (3) extract remainder, add 8 times of water gagings, 100 ℃ decoct 2h, filter and collect the water extract; The water extract is concentrated into 1/8 of original volume; Add the absolute ethyl alcohol of 5 times of amounts after the cooling, stir, 2 ℃ of airtight refrigeration 12h; Centrifugal 10min under the 3500r/min condition then, separate throw out; In throw out, add 5 times of amount 80% ethanol again, stir, the centrifugal 10min of 3500r/min is deposited in 60 ℃ of dry polysaccharides from ginkgo biloba that get.
The filtrating of (5) step (2) being collected is passed through the ultra-fine filter of molecular weight cut-off 10000D, uses the sulfonated polyether sulfone flat plate ultrafiltration membrane, and the control ultrafiltration pressure is 0.25MPa; 28 ℃ of ultrafiltration repeatedly of temperature when the trapped fluid volume reduces to 1/l0, add 75% ethanol of 5 times of volumes; Continue ultrafiltration, when the trapped fluid volume be reduced to once more original volume 1/10 the time, stop ultrafiltration; Collect the ultrafiltration filtered solution, 45 ℃ of vacuum decompressions are concentrated into the liquid concentrator volume: Ginkgo Leaf crude drug=1: 1 (ml: g).
(6) liquid concentrator is adopted supercritical CO
2The equipment extraction, extraction kettle 24 L, extraction kettle pressure 14MPa, 38 ℃ of extraction temperature; 35 ℃ of separation temperatures, I level separating still pressure 9MPa, II level separating still pressure 6MPa, CO
2Flow velocity 1.7L/min (food grade, purity>=99.5%) extracts 40 min, collects extract and gets the separating Ginkgo phenolic acids alcohol mixeding liquid.The water that adds 5 times of volumes in the extract stirs 1 ℃ of airtight refrigeration 12h; Centrifugal 10min under the 3500r/min condition then, collecting precipitation gets the ginkgolic acid compounds.
(7) extraction conditions is adjusted into: extraction kettle pressure 25MPa, 46 ℃ of extraction temperature are launched rectifying volumn (dividing four-section ladder degree temperature control), set to be followed successively by from the temperature to capital at the bottom of the post: 45 ℃, 50 ℃, 55 ℃, 60 ℃; 40 ℃ of separation temperatures, separating still pressure 6MPa continues extraction 60 min, and 0-20 min collects extract and gets ginkgo terpene lactone ethanolic soln, and 20-60 min collects extract and gets ginkgolic flavone glycoside class ethanolic soln; Being concentrated into specific density in 45 ℃ of vacuum decompressions is 1.15 (40 ℃), and the liquid concentrator vacuum lyophilization gets ginkgo terpene lactone, flavonoid compound respectively.
Embodiment 2: Ginkgo Leaf component separating resulting
Each component that embodiment 1 obtains is carried out check and analysis, and its compound quality, purity, percentage extraction are seen table 1.
Table 1 Ginkgo Leaf component separating resulting
The above is merely preferred embodiment of the present invention, and all equalizations of doing according to claim of the present invention change and modify, and all should belong to covering scope of the present invention.
Claims (4)
1. multi-component stripping technique of Ginkgo Leaf, it is characterized in that: described stripping technique comprises following steps:
(1) get Ginkgo Leaf and carry out pre-treatment: removal of impurities also is dried to water ratio≤5%, pulverizes the 10-24 mesh sieve;
(2) ethanolic soln of Ginkgo Leaf being put into the 75-90% of 10-12 times of weight floods 60-90min, and the power ultrasonic with 3000-4000W under 40-45 ℃ condition extracts the 30-40min after-filtration; With the ethanolic soln supersound extraction of the 60-75% of 10-12 times of weight, condition is the same again for filter residue, filters, and merges filtrate for later use twice;
(3) filter residue with step (2) adopts supercritical CO
2Extraction, condition is: extraction kettle pressure is 25-30MPa, extraction temperature is 50-55 ℃; Separation temperature is 40 ℃, and I level separating still pressure is 8-10MPa, and II level separating still pressure is 6MPa, CO
2Flow velocity is 2-2.5L/min, and the extraction time is 4-5h, and separating still is collected and obtained polypenthylene alcohols oily matter, and extract remainder is subsequent use;
(4) add the water of 10-12 times of weight in the extract remainder of step (3), 100 ℃ decoct 2h, filter and collect the water extract; The water extract is concentrated into the 1/8-1/l0 of original volume; The cooling back adds the absolute ethyl alcohol of 5 times of volumes, stirs 1-4 ℃ of airtight refrigeration 12h; Centrifugal 8-10min under the 3000-4000r/min condition then, separate throw out; Add 80% ethanolic soln of 10-12 times of weight again in the throw out, stir, with the centrifugal 8-10min of 3000-4000r/min, deposition, vacuum lyophilization get polysaccharides from ginkgo biloba;
The filtrating of (5) step (2) being collected is the ultra-fine filter of 10000D through molecular weight cut-off, adopts the sulfonated polyether sulfone flat plate ultrafiltration membrane, and the control ultrafiltration pressure is 0.20~0.25MPa; Temperature is 25-30 ℃ and carries out ultrafiltration repeatedly; When the trapped fluid volume reduces to 1/l0, add 75% ethanolic soln of 5 times of volumes, continue ultrafiltration; When the trapped fluid volume be reduced to once more original volume 1/10 the time; Stop ultrafiltration, collect the ultrafiltration filtered solution, 45-50 ℃ of vacuum decompression is concentrated into the liquid concentrator volume and Ginkgo Leaf raw materials quality ratio is 1: 1;
(6) liquid concentrator with step (5) adopts supercritical CO
2The equipment extraction, condition is: extraction kettle pressure is 10-16MPa, extraction temperature is 35-40 ℃; Separation temperature is 35 ℃, and I level separating still pressure is 8-10MPa, and II level separating still pressure is 6MPa, CO
2Flow velocity is 1.5-2L/min, and the extraction time is 30-45 min, collects extract separating Ginkgo phenolic acids alcohol mixeding liquid; Add the water of 5 times of volumes in the extract, stir 1-4 ℃ of airtight refrigeration 12h; Then with the centrifugal 8-10min of 3000-4000r/min, collecting precipitation ginkgolic acid compounds;
(7) extraction conditions is adjusted into: extraction kettle pressure is 20-28MPa, and extraction temperature is 45-50 ℃, launches rectifying volumn, divides four-section ladder degree temperature control, sets to be followed successively by from the temperature to capital at the bottom of the post: 45 ℃, 50 ℃, 55 ℃, 60 ℃; Separation temperature is 40 ℃; Separating still pressure is 5-8MPa; Continue extraction 50-70 min, collect extract at times, obtain ginkgo terpene lactone and flavonoid ethanolic soln respectively; Specific density when 45-50 ℃ of vacuum decompression is concentrated into 40 ℃ is 1.10-1.20, and the liquid concentrator vacuum lyophilization gets ginkgo terpene lactone and flavonoid compound respectively;
More than filtering and all adopting the order number is 200-300 purpose screen cloth; Alcohol concn described in step (2), (4) and (5) is volume percent; CO described in step (3) and (6)
2Be food grade, purity>=99.5%.
2. the multi-component stripping technique of Ginkgo Leaf according to claim 1 is characterized in that: the Ginkgo Leaf in the step (1) is to pluck in the 2-3 age of tree, 5-7 month.
3. the multi-component stripping technique of Ginkgo Leaf according to claim 1 is characterized in that: extracting the alcohol concn that uses for the first time in the step (2) is 85%, and extracting the alcohol concn that uses for the second time is 70%; Described alcohol concn is volume percent.
4. the multi-component stripping technique of Ginkgo Leaf according to claim 1 is characterized in that: extraction kettle pressure is 14MPa in the step (6), and extraction temperature is 38 ℃; Separation temperature is 35 ℃, and I level separating still pressure is 9MPa, and II level separating still pressure is 6MPa, CO
2Flow velocity is 1.8L/min, and the extraction time is 45 min; Described CO
2Be food grade, purity>=99.5%.
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Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103044378A (en) * | 2012-12-31 | 2013-04-17 | 浙江大学宁波理工学院 | Method for extracting ginkgetin from leaves of taxus mairei |
CN103130816A (en) * | 2012-10-19 | 2013-06-05 | 湖北诺克特药业有限公司 | Method of preparing a plurality of active substances from ginkgo leaves |
CN103739612A (en) * | 2013-12-26 | 2014-04-23 | 哈尔滨誉衡药业股份有限公司 | Traditional Chinese medicine raw material |
CN105477026A (en) * | 2016-02-02 | 2016-04-13 | 武汉理工大学 | Process for extracting ginkgolic acid, flavone, terpene lactones and polysaccharose from gingko exotesta in combined mode |
CN105853474A (en) * | 2016-06-14 | 2016-08-17 | 南京华宽信息咨询中心 | Ginkgolide extracting method and ginkgolide extract |
CN106421511A (en) * | 2016-12-28 | 2017-02-22 | 四川默森药业有限公司 | Aloe antibacterial composition and preparation method thereof |
CN106727738A (en) * | 2016-12-14 | 2017-05-31 | 四川岚晟生物科技有限公司 | A kind of Phellinus glossy ganoderma powder and preparation method thereof |
CN106822196A (en) * | 2017-03-23 | 2017-06-13 | 山东天智绿业生物科技有限公司 | A kind of method for extracting Ginkgo biloba polysaccharide and ginko leaves flavone simultaneously from ginkgo leaf |
CN107760058A (en) * | 2017-11-30 | 2018-03-06 | 广西南宁栩兮科技有限公司 | The extracting method of haematochrome in a kind of rambutan shell |
CN112998064A (en) * | 2021-04-25 | 2021-06-22 | 福建省农通科技发展有限公司 | Preservative and preparation method thereof |
CN114196479A (en) * | 2021-12-31 | 2022-03-18 | 广西膳君特医食品有限公司 | Low-temperature extraction process of ginkgo leaves |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1392167A (en) * | 2001-06-18 | 2003-01-22 | 中国林业科学研究院林产化学工业研究所 | Preparing process and use of ginkgo leaf polypentenol and ginkgo leaf extract |
-
2012
- 2012-02-20 CN CN2012100381038A patent/CN102603482B/en not_active Expired - Fee Related
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1392167A (en) * | 2001-06-18 | 2003-01-22 | 中国林业科学研究院林产化学工业研究所 | Preparing process and use of ginkgo leaf polypentenol and ginkgo leaf extract |
Non-Patent Citations (2)
Title |
---|
侯峰等: "超临界CO2脱除银杏叶提取物中酚酸的研究", 《中草药》, vol. 34, no. 1, 31 January 2003 (2003-01-31), pages 37 - 39 * |
张富捐: "银杏叶活性成分的提取与研究进展", 《许昌师专学报》, vol. 21, no. 5, 30 September 2002 (2002-09-30), pages 18 - 22 * |
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CN103130816A (en) * | 2012-10-19 | 2013-06-05 | 湖北诺克特药业有限公司 | Method of preparing a plurality of active substances from ginkgo leaves |
CN103044378B (en) * | 2012-12-31 | 2015-04-22 | 浙江大学宁波理工学院 | Method for extracting ginkgetin from leaves of taxus mairei |
CN103044378A (en) * | 2012-12-31 | 2013-04-17 | 浙江大学宁波理工学院 | Method for extracting ginkgetin from leaves of taxus mairei |
CN103739612A (en) * | 2013-12-26 | 2014-04-23 | 哈尔滨誉衡药业股份有限公司 | Traditional Chinese medicine raw material |
CN105477026B (en) * | 2016-02-02 | 2019-10-01 | 武汉理工大学 | A kind of technique of combined extracting ginkgoic acid, flavones and terpene lactones and polysaccharide from gingko episperm |
CN105477026A (en) * | 2016-02-02 | 2016-04-13 | 武汉理工大学 | Process for extracting ginkgolic acid, flavone, terpene lactones and polysaccharose from gingko exotesta in combined mode |
CN105853474A (en) * | 2016-06-14 | 2016-08-17 | 南京华宽信息咨询中心 | Ginkgolide extracting method and ginkgolide extract |
CN106727738A (en) * | 2016-12-14 | 2017-05-31 | 四川岚晟生物科技有限公司 | A kind of Phellinus glossy ganoderma powder and preparation method thereof |
CN106421511A (en) * | 2016-12-28 | 2017-02-22 | 四川默森药业有限公司 | Aloe antibacterial composition and preparation method thereof |
CN106822196A (en) * | 2017-03-23 | 2017-06-13 | 山东天智绿业生物科技有限公司 | A kind of method for extracting Ginkgo biloba polysaccharide and ginko leaves flavone simultaneously from ginkgo leaf |
CN106822196B (en) * | 2017-03-23 | 2020-07-07 | 山东天智绿业生物科技有限公司 | Method for simultaneously extracting ginkgo leaf polysaccharide and ginkgo leaf flavone from ginkgo leaves |
CN107760058A (en) * | 2017-11-30 | 2018-03-06 | 广西南宁栩兮科技有限公司 | The extracting method of haematochrome in a kind of rambutan shell |
CN112998064A (en) * | 2021-04-25 | 2021-06-22 | 福建省农通科技发展有限公司 | Preservative and preparation method thereof |
CN114196479A (en) * | 2021-12-31 | 2022-03-18 | 广西膳君特医食品有限公司 | Low-temperature extraction process of ginkgo leaves |
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