CN1472206A - Method for preparing ginkgo leaf extractive - Google Patents
Method for preparing ginkgo leaf extractive Download PDFInfo
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- CN1472206A CN1472206A CNA021344906A CN02134490A CN1472206A CN 1472206 A CN1472206 A CN 1472206A CN A021344906 A CNA021344906 A CN A021344906A CN 02134490 A CN02134490 A CN 02134490A CN 1472206 A CN1472206 A CN 1472206A
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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
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Abstract
A process for preparing the extract of ginkgo leaf includes such steps as pulverizing ginkgo leaves, immersing in alcohol, concentrating, depositing in wine, refining ginkgo flavone from supernatant by macroreticular resin method, refining ginkgo lactone from deposit by supercritical CO2 method, and proportionally mixing them together. Its advantages are low cost, high purity and stability, and high output rate (more than 80%).
Description
Technical field
The present invention relates to process for extracting to flavones in the Ginkgo Leaf and lactone composition.
Background technology
Folium Ginkgo extract has the cardiovascular and cerebrovascular circulation of improvement, and the treatment cardiovascular and cerebrovascular diseases improves memory, removes oxyradical, and function in delaying senility has treatment and health care double effects.Its effective constituent is ginkgolic flavone glycoside and lactone, and its content height and relative proportion determine the quality of its quality.The preparation technology who extracts Folium Ginkgo extract at present from Ginkgo Leaf has: 1, water is taken out method, comprising: A, water extracting-ethanol precipitation, B, water extracting-resin method; 2, ethanol extraction process; 3, acetone extraction process etc.These methods extract ginkgolic flavone glycoside and lactone simultaneously, be subjected to weather, the place of production, acquisition time, deposit factor affecting such as phase because of the Ginkgo Leaf quality again, the content instability, above technology is difficult to guarantee that the flavones in the extract and the content of lactone all reach the relatively stable of quality index and flavones and lactone ratio, therefore is difficult to produce high-quality Folium Ginkgo extract.
Summary of the invention
The objective of the invention is to propose the novel preparation method of the stable Folium Ginkgo extract of a kind of content that is intended to obtain to have ginkgolic flavone glycoside and lactone and relative proportion.
The present invention adopts ethanol slightly to carry-Amberlyst process and supercritical CO
2Extract the technical scheme of purifying-blend, be about to Ginkgo Leaf and pulverize back ethanol lixiviate, it is heavy that extract concentrates back wine, and supernatant layer is used for refining ginkgolic flavone glycoside, and throw out is used for making with extra care bilobalide; Adopt the refining ginkgolic flavone glycoside of Amberlyst process, supercritical CO
2Method is made with extra care bilobalide, make ginkgolic flavone glycoside and bilobalide extract respectively, on the basis of the content of the ginkgolic flavone glycoside of measuring extract and bilobalide, blend then to mix and have the Folium Ginkgo extract that ginkgolic flavone glycoside and bilobalide are stablized content and proportioning.Its concrete processing step is:
(1) extract ginkgo effective constituent,
(1.1), the ginkgo cured leaf pulverized after, add the ethanol lixiviate, vat liquor, condition is: extraction temperature is 60-80 ℃, alcohol concn is 65-75%;
(1.2), the vat liquor filtration final vacuum with gained is condensed into concentrated solution;
(1.3), add the concentrated solution of gained with acid to be that the ethanol of 5-20% is adjusted to the acid ethanol solution that the pH value is 2-5 with concentration, to leave standstill, it is fully precipitated, filtration, supernatant liquor and throw out is separately standby;
(2) extract ginkgolic flavone glycoside,
(2.1), the supernatant liquor of (1.3) gained is crossed macroporous resin column;
(2.2), supernatant liquor is used the drip washing of 65-75% aqueous ethanolic solution after crossing post, the collection effluent liquid;
(2.3), with behind the effluent liquid decompression recycling ethanol of collecting, vacuum spray drying and gingko flavone extractive;
(3) extract bilobalide,
(3.1), the throw out of (1.3) gained adds sorbent material.Sorbent material can be polymeric amide, diatomite or macroporous resin.Sorbent material is best with the polymeric amide.
(3.2) will go up throw out that the step the is added with sorbent material supercritical CO of packing into
2Extraction kettle carries out supercritical CO
2Extraction, the extraction process condition is: extraction temperature is 45-60 ℃, and extracting pressure is 20-40Mpa, carrying agent is 50-80% ethanol; Its optimum process condition is: extraction temperature is 55 ℃, and extracting pressure is 25Mpa, and carrying agent is 70% ethanol.
(3.3), behind the extract concentrating under reduced pressure with gained, vacuum spray drying and the bilobalide extract;
(4), make general flavone content 〉=24% in the Folium Ginkgo extract product after the allotment, total lactone 〉=6% respectively to the gingko flavone extractive and the weighing of bilobalide extract of gained and blend allotment.
The inventive method can guarantee to make has the high-quality Folium Ginkgo extract that ginkgolic flavone glycoside and bilobalide are stablized content and proportioning, be not subjected to the influence of the quality factor of Ginkgo Leaf own, prepare the existing problem of Folium Ginkgo extract thereby solved existing Ginkgo Leaf extraction process.This law technology is simple, and production cost is low, prepared Folium Ginkgo extract general flavone content 〉=24%, total lactone 〉=6%, steady quality; The rate of recovery 〉=80%.
Description of drawings
Accompanying drawing is a supercritical CO
2The extracting system synoptic diagram.
Among the figure: 1 is CO
2Gas cylinder, 2 is refrigerated tank, and 3 for carrying the agent jar, and 4 is under meter, and 5 is high-pressure pump, and 6 is volume pump, and 7 is extraction kettle, and 8,9,10 is separating still, 11,12,13,14,15,16,17,18,19,20,21,22,23,24,25,26 is valve.
Specific embodiments
The processing step of preparation Semen Ginkgo extrac is as follows:
(1) extract ginkgo effective constituent,
(1.1), with after the pulverizing of ginkgo cured leaf, be put in the water-bath, branch adds 5 times, 4 times, 3 times the ethanol that is respectively ginkgo cured leaf weight for three times Ginkgo Leaf is distinguished lixiviate 3 hours, 2 hours, 1 hour, extraction temperature is 70 ℃, alcohol concn is 75%, after each lixiviate, collect extracting solution, with the extracting solution merging of three collections;
(1.2), the vat liquor filtration final vacuum with gained is condensed into concentrated solution;
(1.3), the concentrated solution of gained is added acid ethanol solution, this acidic solution for hydrochloric acid with concentration be 15% ethanol to be adjusted to pH value be 3 ethanolic soln, left standstill 10 hours, it is fully precipitated, filtration, supernatant liquor and throw out is separately standby;
(2) extract ginkgolic flavone glycoside,
(2.1), the supernatant liquor of (1.3) gained is crossed macroporous resin column, process is as follows: a, earlier to the macroporous resin pre-treatment, getting granularity is 30-60 purpose AB-8 resin, soak 24 hours after, used 5% soaking with sodium hydroxide again 4 hours, with distilled water flushing near neutral; Added 5% salt acid soak again 4 hours, extremely near neutral with distilled water flushing; Add 95% alcohol immersion again after 8 hours, standby when being washed till no ethanol flavor repeatedly with distilled water; B, with the resin of handling well the glass chromatography column of packing into, dash to balance with distilled water, then the supernatant liquor of (1.3) gained is crossed post, regulate the about 60/min of flow velocity, after treating that solution has all been crossed, when effluent liquid becomes brown clear liquor by green turbid solution, enter next step with 15% ethanol (pH=3) drip washing and collect step;
(2.2), with 75% aqueous ethanolic solution (pH=3) drip washing, collect effluent liquid, until effluent liquid become limpid till;
(2.3), with behind the effluent liquid decompression recycling ethanol of collecting, vacuum spray drying promptly gets gingko flavone extractive;
(3) extract bilobalide,
(3.1), use supercritical CO
2Extracting process (is used supercritical CO shown in the drawings to the throw out extraction bilobalide of (1.3) gained
2Extracting system), its technical process is: the throw out of (1.3) gained is added sorbent material polymeric amide, the supercritical CO of packing into
2Extraction kettle 7 after extraction kettle 7 is heated to 55 ℃ of extraction temperature, feeds liquid CO to extraction kettle
2Ethanol with carrying agent (extraction agent) 70% concentration circulates under the 25Mpa extracting pressure, extracts after 1 hour, obtains thick shape cream at separating still 8, obtains the darker solution of color at separating still 9, obtains more clear solution in separating still collection 10.The solution meridian film that obtains from separating still 9 obtains thick shape medicinal extract after concentrating, this medicinal extract with obtain thick shape cream from separating still 8 and merge that to be the bilobalide extract standby to enter the subsequent processing step.The solution of separating still 10 gained can add extraction kettle to be reused, and the temperature of said separating still 8,9,10 is adjusted to 60 ℃, 45 ℃, 40 ℃ respectively.
(3.2), will go up the step gained bilobalide extract concentrating under reduced pressure after, vacuum spray drying and the bilobalide extract;
(4) respectively the gingko flavone extractive and the bilobalide extract of gained are measured its ginkgolic flavone glycoside and bilobalide content with the HPLC method respectively, by general flavone content 〉=24% in the Folium Ginkgo extract product after the allotment, total lactone 〉=6% is a standard, to the weighing and blend allotment respectively of gingko flavone extractive and bilobalide extract, promptly obtain Folium Ginkgo extract product of the present invention.
Claims (2)
1. the preparation method of a Folium Ginkgo extract, its processing step is:
(1) extract ginkgo effective constituent,
(1.1), the ginkgo cured leaf pulverized after, add the ethanol lixiviate, vat liquor, condition is: extraction temperature is 60-80 ℃, alcohol concn is 65-75%;
(1.2), the vat liquor filtration final vacuum with gained is condensed into concentrated solution;
(1.3), add the concentrated solution of gained with acid to be that the ethanol of 5-20% is adjusted to the acid ethanol solution that the pH value is 2-5 with concentration, to leave standstill, it is fully precipitated, filtration, supernatant liquor and throw out is separately standby;
(2) extract ginkgolic flavone glycoside,
(2.1), the supernatant liquor of (1.3) gained is crossed macroporous resin column;
(2.2), supernatant liquor is used the drip washing of 65-75% aqueous ethanolic solution after crossing post, the collection effluent liquid;
(2.3), with behind the effluent liquid decompression recycling ethanol of collecting, vacuum spray drying and gingko flavone extractive;
(3) extract bilobalide,
(3.1), the throw out of (1.3) gained adds sorbent material;
(3.2), will go up throw out that the step the is added with sorbent material supercritical CO of packing into
2Extraction kettle carries out supercritical CO
2Extraction, the extraction process condition is: extraction temperature is 45-60 ℃, and extracting pressure is 20-40Mpa, carrying agent is 50-80% ethanol;
(3.3), behind the extract concentrating under reduced pressure with gained, vacuum spray drying and the bilobalide extract;
(4), make general flavone content 〉=24% in the Folium Ginkgo extract product after the allotment, total lactone 〉=6% respectively to the gingko flavone extractive and the weighing of bilobalide extract of gained and blend allotment.
2. the preparation method of Folium Ginkgo extract according to claim 1 is characterized in that using supercritical CO
2The processing condition that extraction process extracts bilobalide are: extraction temperature is 55 ℃, and extracting pressure is 25Mpa, and carrying agent is 70% ethanol, and sorbent material is a polymeric amide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021344906A CN1211378C (en) | 2002-08-02 | 2002-08-02 | Method for preparing ginkgo leaf extractive |
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| CNB021344906A CN1211378C (en) | 2002-08-02 | 2002-08-02 | Method for preparing ginkgo leaf extractive |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100343375C (en) * | 2005-08-11 | 2007-10-17 | 江苏同源堂生物工程有限公司 | Supercritical carbon dioxide extraction method for extracting gingko oil from gingko fruit |
| CN100446778C (en) * | 2007-04-18 | 2008-12-31 | 黑龙江省珍宝岛制药有限公司 | Method of preparing solution / substance extracted from ginkgo leaves |
| CN100469774C (en) * | 2006-04-13 | 2009-03-18 | 厦门国宇知识产权研究有限公司 | Ginkgo leaf extract and production process of separating high purity effective component of the extract |
| CN1830981B (en) * | 2006-04-17 | 2010-05-12 | 四川科伦药业股份有限公司 | Injection emulsion for treating cerebrovascular disease and its preparing process |
| CN102488721A (en) * | 2011-12-14 | 2012-06-13 | 广东长兴科技保健品有限公司 | Preparation method for ginkgo leaf extracts and preparation of ginkgo leaf extracts |
| CN105641003A (en) * | 2015-08-21 | 2016-06-08 | 徐州市大药上德生物科技有限公司 | Natural plant extract and applications thereof |
| CN106038619A (en) * | 2016-06-08 | 2016-10-26 | 河南骏化发展股份有限公司 | Ginkgo biloba leaf extract and preparation method thereof |
| CN107647407A (en) * | 2017-11-14 | 2018-02-02 | 宜昌东方昌绿茶业有限公司 | A kind of method that flavonol is extracted from ginkgo leave tea |
-
2002
- 2002-08-02 CN CNB021344906A patent/CN1211378C/en not_active Expired - Lifetime
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100343375C (en) * | 2005-08-11 | 2007-10-17 | 江苏同源堂生物工程有限公司 | Supercritical carbon dioxide extraction method for extracting gingko oil from gingko fruit |
| CN100469774C (en) * | 2006-04-13 | 2009-03-18 | 厦门国宇知识产权研究有限公司 | Ginkgo leaf extract and production process of separating high purity effective component of the extract |
| CN1830981B (en) * | 2006-04-17 | 2010-05-12 | 四川科伦药业股份有限公司 | Injection emulsion for treating cerebrovascular disease and its preparing process |
| CN100446778C (en) * | 2007-04-18 | 2008-12-31 | 黑龙江省珍宝岛制药有限公司 | Method of preparing solution / substance extracted from ginkgo leaves |
| CN102488721A (en) * | 2011-12-14 | 2012-06-13 | 广东长兴科技保健品有限公司 | Preparation method for ginkgo leaf extracts and preparation of ginkgo leaf extracts |
| CN102488721B (en) * | 2011-12-14 | 2013-07-31 | 广东长兴生物科技股份有限公司 | Preparation method for ginkgo leaf extracts and preparation of ginkgo leaf extracts |
| CN105641003A (en) * | 2015-08-21 | 2016-06-08 | 徐州市大药上德生物科技有限公司 | Natural plant extract and applications thereof |
| CN106038619A (en) * | 2016-06-08 | 2016-10-26 | 河南骏化发展股份有限公司 | Ginkgo biloba leaf extract and preparation method thereof |
| CN106038619B (en) * | 2016-06-08 | 2019-08-23 | 河南骏化发展股份有限公司 | A kind of ginkgo biloba p.e and preparation method thereof |
| CN107647407A (en) * | 2017-11-14 | 2018-02-02 | 宜昌东方昌绿茶业有限公司 | A kind of method that flavonol is extracted from ginkgo leave tea |
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| CN1211378C (en) | 2005-07-20 |
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Owner name: SHANXI ZHENDONGTAISHENG PHARMACEUTICAL CO., LTD. Free format text: FORMER OWNER: GUANGDONG TESTING AND ANALYSIS INST. Effective date: 20100927 |
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Effective date of registration: 20100927 Address after: 037300 No. 56 Hubin street, Datong economic and Technological Development Zone, Shanxi Patentee after: SHANXI ZHENDONG TAISHENG PHARMACEUTICAL Co.,Ltd. Address before: Guangzhou City, Guangdong province 510070 martyrs Road No. 100 Patentee before: GUANGDONG INSTITUTE OF ANALYSIS |
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