CN103159779A - Industrialization production technology for extracting bilobalide from Ginkgo testa - Google Patents
Industrialization production technology for extracting bilobalide from Ginkgo testa Download PDFInfo
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- CN103159779A CN103159779A CN2011104194017A CN201110419401A CN103159779A CN 103159779 A CN103159779 A CN 103159779A CN 2011104194017 A CN2011104194017 A CN 2011104194017A CN 201110419401 A CN201110419401 A CN 201110419401A CN 103159779 A CN103159779 A CN 103159779A
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- bilobalide
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- gingko episperm
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Abstract
The invention relates to an industrialization production technology for extracting bilobalide from Ginkgo testa. The technology comprises the following steps: leaching Ginkgo testa; separating, concentrating and fractionating leaching extracts; adjusting a pH value of the concentrated liquid; isolating a crude extract of ginkgolic acid; extracting a filtered mother liquor, conducting back extraction and adjusting the pH value; acidifying, concentrating, cooling and filtering to obtain a bilobalide crude product; dissolving the crude product with ethanol; and conducting column separation to obtain bilobalide with high purity. The invention employs ginkgolide acid solution to regulate the pH value of the solution containing bilobalide, and precipitates the bilobalide by a common ion effect. The technology has the advantages of simple process, convenient operation, low cost, high extraction rate and high extraction purity, can rapidly extract bilobalide in large amount from Ginkgo testa, and is suitable for requirements of industrial production.
Description
Technical field
The present invention relates to the comprehensive utilization of gingko episperm, is a kind of Industrialized processing technique that extracts bilobalide from gingko episperm specifically.
Background technology
Ginkgo is China's endemic tree, is also important economic plants, and this not only has the title of living fossil, and more having is the what is said or talked about of treasured from head to foot.The developed countries such as in recent years, ginkgo and related products thereof are more and more paid attention in the international market, and be American-European have all carried out deep development to it, in succession develop multiple medicine, and healthcare products and makeup are made a profit considerable.China also payes attention to all the more on to the comprehensive utilization of ginkgo nut, Ginkgo Leaf.Yet the gingko episperm that accounts for the most of weight of ginkgo fruit generally abandons when waste, fails to be fully used, simultaneously to environment.
After deliberation, in gingko episperm the substances content such as contained ginkgoic acid, bilobalide be the contained 2-3 of ginkgo nut or Ginkgo Leaf doubly, have to extract and be worth.Bilobalide has vasodilation, increases volume of blood flow, improves microcirculation, removes free radical, antianaphylaxis, anti-inflammatory, the effectiveness such as antitumor, can be used as the specifics of cardiovascular and cerebrovascular diseases, and its structure is:
The extractive technique of gingko episperm all there is relevant report both at home and abroad.At present, extracting method commonly used is organic solvent extraction method, supercritical CO
2Extraction method, water extraction one resin method, gush out chromatographic technique extraction method, cell tissue cultivated synthetic extraction method, resin extraction method, enzyme extraction method etc. at a high speed, because R base kind on bilobalide is more, the said extracted method is only suitable for extracting for the bilobalide of certain single kind, its extraction process complexity is loaded down with trivial details, operational requirement is high, the time is long, cost is high, can't apply in industrialized production.
Summary of the invention
To extract bilobalide in gingko episperm and can't be applicable to drawback in industrialized production in order to solve in prior art, the invention provides a kind of technique simple, easy to operate, production cost is low, extraction yield is high, extraction accuracy is high, can satisfy the Industrialized processing technique that extracts bilobalide from gingko episperm of industrialized production requirement.
The technical solution used in the present invention is: a kind of Industrialized processing technique that extracts bilobalide from gingko episperm is characterized in that comprising the following steps:
(1) gingko episperm after cleaning is ground to carefully, crosses the 30-80 order, adds in weight 5-10 water doubly, stirs and soaks 5-12 hour;
(2) the mixed solution centrifugation after soaking is removed slag, and filtrate is pumped in concentrating pan, and vacuum fractionation is concentrated;
(3) add acid solution in solution after concentrated and regulate pH value to 2-3, be cooled to-5-10 ℃, separate out brown crystal, suction filtration;
(4) filtrate in step (3) is extracted with extraction agent, get organic phase and strip with liquid caustic soda, the water after stripping is regulated pH value to 3-5 with acid solution;
(5) solution after step (4) acidifying is concentrated, be cooled to-5-10 ℃ crystallization, filter to get the bilobalide crude product;
(6) carry out post after step (5) bilobalide crude product is fully dissolved with alcoholic solution and separate, can obtain highly purified bilobalide.
Described step (2) vacuum fractionation is concentrated, the component of fractionation 48-70 ℃ under the vacuum tightness of 0.08-0.09Mpa.
In described step (3), (4), acid solution is any one or two or more mixing solutions in hydrochloric acid, phosphoric acid, sulfuric acid, vinyl acetic monomer, oxalic acid, and acid solutions is 10-30%.
In described step (4), (5), alcoholic solution is ethanol or methyl alcohol or both mixing solutionss, solvent temperature 50-70 ℃.
In described step (4), liquid caustic soda is sodium hydroxide or potassium hydroxide or both mixing solutionss, and liquid caustic soda concentration is 10-30%.
Described step (3) suction filtration gets the ginkgoic acid of 60-70%.
In described step (4), extraction agent is sherwood oil or vinyl acetic monomer, and Solvent quantity is 1/3-1/2 mother liquor volume, extracts 2-3 time.
Described step (1) exosper replaces water soaking with 95% ethanol, and the weight of 95% ethanol is 3-5 times of exosper, and stirring soak time is 3-6 hour.
Compared with prior art, the present invention has the following advantages:
1, the solution that contains bilobalide in step (4), (5) is slightly acidic, be highly acid acid solution generation common-ion effcet by adding, regulate pH value and solution temperature, separate out and be weakly acidic bilobalide, realize a large amount of separation of bilobalide, compare in the biological extraction technology factors such as equipment and environmental requirement, extracted amount and costs, have easy to operately, technique is simple, and is low to equipment and environmental requirement, extraction yield is high, advantage with low cost;
2, step (6) adopts alcoholic solution that the bilobalide of crude product is washed, and can effectively improve the purity of bilobalide;
3, in step (2), vacuum fractionation is concentrated, the component of fractionation 48-70 ℃ under the vacuum tightness of 0.08-0.09Mpa, this component is the mixing solutions of ginkgol, ginkgoic acid, butyric acid, sad and water, this mixing solutions tool is better to insect insect killing effects such as aphid, rice borer, mulberry locusts, the effect of good prevention and elimination of disease and pests is arranged, have simultaneously the bacteriostasis, preservation effect, can directly be used as desinsection, antiseptic-germicide, preservation agent, further improve the exosper utility value;
4, adopt the acid solutions such as hydrochloric acid, phosphoric acid, sulfuric acid, vinyl acetic monomer, oxalic acid, the alcoholic solutions such as ethanol or methyl alcohol, the liquid caustic soda such as sodium hydroxide or potassium hydroxide, commercial acid, alkali are as the raw material commonly used of suitability for industrialized production, and use cost is low, can repeat to reclaim and use.
The present invention utilizes acid solution to regulate the pH value of bilobalide-containing solution, by common-ion effcet, bilobalide is separated out, this technology has that technique is simple, easy to operate, cost is low, extraction yield is high, the advantage that DNA purity is high, can in a large number, promptly extract bilobalide from the ginkgo exterior skin, be fit to the requirement of industrialized production.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment one
A kind of Industrialized processing technique that extracts bilobalide from gingko episperm is characterized in that comprising the following steps:
(1) gingko episperm after cleaning is ground to carefully, crosses 30 orders, adds in the water of 5 times of weight, stirs and soaks 5 hours;
(2) the mixed solution centrifugation after soaking is removed slag, and filtrate is pumped in concentrating pan, and vacuum fractionation goes out the component of 48 ℃ under the vacuum tightness of 0.08Mpa, and concentrated;
(3) adding concentration in solution after concentrated is that 10% hydrochloric acid is regulated pH value to 3, is cooled to 10 ℃, separates out brown crystal, the suction filtration brown crystal;
(4) filtrate in step (3) is extracted with sherwood oil, Solvent quantity is 1/3 mother liquor volume, extracts 2 times; Getting organic phase concentration is that 10% sodium hydroxide is stripped, and is that 10% hydrochloric acid is regulated pH value to 5 with the water concentration after stripping;
(5) solution after step (4) acidifying is concentrated, be cooled to-5 ℃ of crystallizations, filter to get the bilobalide crude product;
(6) step (5) bilobalide crude product is fully carried out the post separation after dissolving with 50 ℃ of ethanol intensifications, can obtain highly purified bilobalide.
Embodiment two
A kind of Industrialized processing technique that extracts bilobalide from gingko episperm is characterized in that comprising the following steps:
(1) gingko episperm after cleaning is ground to carefully, crosses 60 orders, adds in the water of 8 times of weight, stirs and soaks 8 hours;
(2) the mixed solution centrifugation after soaking is removed slag, and filtrate is pumped in concentrating pan, and vacuum fractionation goes out the component of 60 ℃ under the vacuum tightness of 0.085Mpa, and concentrated;
(3) adding concentration in solution after concentrated is that 20% hydrochloric acid is regulated pH value to 2.5, is cooled to 2 ℃, separates out brown crystal, the suction filtration brown crystal;
(4) filtrate in step (3) is extracted with sherwood oil, Solvent quantity is 5/12 mother liquor volume, extracts 2 times; Getting organic phase concentration is that 20% sodium hydroxide is stripped, and is that 20% hydrochloric acid is regulated pH value to 4 with the water concentration after stripping;
(5) solution after step (4) acidifying is concentrated, be cooled to 4 ℃ of crystallizations, filter to get the bilobalide crude product;
(6) step (5) bilobalide crude product is fully carried out the post separation after dissolving with 60 ℃ of ethanol intensifications, can obtain highly purified bilobalide.
Embodiment three
A kind of Industrialized processing technique that extracts bilobalide from gingko episperm is characterized in that comprising the following steps:
(1) gingko episperm after cleaning is ground to carefully, crosses 80 orders, adds in the water of 10 times of weight, stirs and soaks 12 hours;
(2) the mixed solution centrifugation after soaking is removed slag, and filtrate is pumped in concentrating pan, and vacuum fractionation goes out the component of 70 ℃ under the vacuum tightness of 0.09Mpa, and concentrated;
(3) adding concentration in solution after concentrated is that 30% hydrochloric acid is regulated pH value to 2, is cooled to-5 ℃, separates out brown crystal, the suction filtration brown crystal;
(4) filtrate in step (3) is extracted with sherwood oil, Solvent quantity is 1/2 mother liquor volume, extracts 3 times; Getting organic phase concentration is that 30% sodium hydroxide is stripped, and after stripping, water intaking is that 30% hydrochloric acid is regulated pH value to 3 with concentration mutually;
(5) solution after step (4) acidifying is concentrated, be cooled to 10 ℃ of crystallizations, filter to get the bilobalide crude product;
(6) step (5) bilobalide crude product is fully carried out the post separation after dissolving with 70 ℃ of ethanol intensifications, can obtain highly purified bilobalide.
Embodiment four
A kind of Industrialized processing technique that extracts bilobalide from gingko episperm is characterized in that comprising the following steps:
(1) gingko episperm after cleaning is ground to carefully, crosses 80 orders, adds in 95% ethanol of 5 times of weight, stirs and soaks 6 hours;
(2) the mixed solution centrifugation after soaking is removed slag, and filtrate is pumped in concentrating pan, and vacuum fractionation goes out the component of 70 ℃ under the vacuum tightness of 0.09Mpa, and concentrated;
(3) adding concentration in solution after concentrated is that 30% oxalic acid is regulated pH value to 2, is cooled to-5 ℃, separates out brown crystal, the suction filtration brown crystal;
(4) filtrate in step (3) is extracted with vinyl acetic monomer, Solvent quantity is 1/2 mother liquor volume, extracts 3 times; Getting organic phase concentration is that 30% potassium hydroxide is stripped, and is that 30% oxalic acid is regulated pH value to 3 with the water concentration after stripping;
(5) solution after step (4) acidifying is concentrated, be cooled to 10 ℃ of crystallizations, filter to get the bilobalide crude product;
(5) step (5) bilobalide crude product is fully carried out the post separation after dissolving with 70 ℃ of methyl alcohol intensifications, can obtain highly purified bilobalide.
But the bilobalide of the every 1T gingko episperm of the present invention output 1-2Kg ester content 93%, the industrialized utilization rate is higher.
Claims (8)
1. Industrialized processing technique that extracts bilobalide from gingko episperm is characterized in that comprising the following steps:
(1) gingko episperm after cleaning is ground to carefully, crosses the 30-80 order, adds in weight 5-10 water doubly, stirs and soaks 5-12 hour;
(2) the mixed solution centrifugation after soaking is removed slag, and filtrate is pumped in concentrating pan, and vacuum fractionation is concentrated;
(3) add acid solution in solution after concentrated and regulate pH value to 2-3, be cooled to-5-10 ℃, separate out brown crystal, suction filtration;
(4) filtrate in step (3) is extracted with extraction agent, get organic phase and strip with liquid caustic soda, the water after stripping is regulated pH value to 3-5 with acid solution;
(5) solution after step (4) acidifying is concentrated, be cooled to-5-10 ℃ crystallization, filter to get the bilobalide crude product;
(6) carry out post after step (5) bilobalide crude product is fully dissolved with alcoholic solution and separate, get high purity ginkgo lactone.
2. the Industrialized processing technique that extracts bilobalide from gingko episperm according to claim 1, it is characterized in that: described step (2) vacuum fractionation is concentrated, the component of fractionation 48-70 ℃ under the vacuum tightness of 0.08-0.09Mpa.
3. the Industrialized processing technique that extracts bilobalide from gingko episperm according to claim 1, it is characterized in that: in described step (3), (4), acid solution is any one or two or more mixing solutions in hydrochloric acid, phosphoric acid, sulfuric acid, vinyl acetic monomer, oxalic acid, and acid solutions is 10-30%.
4. the Industrialized processing technique that extracts bilobalide from gingko episperm according to claim 1, it is characterized in that: in described step (4), (6), alcoholic solution is ethanol or methyl alcohol or both mixing solutionss, solvent temperature 50-70 ℃.
5. the Industrialized processing technique that extracts bilobalide from gingko episperm according to claim 1, it is characterized in that: in described step (4), liquid caustic soda is sodium hydroxide or potassium hydroxide or both mixing solutionss, and liquid caustic soda concentration is 10-30%.
6. the Industrialized processing technique that extracts bilobalide from gingko episperm according to claim 1, it is characterized in that: described step (3) suction filtration gets the ginkgoic acid of 60-70%.
7. the Industrialized processing technique that extracts bilobalide from gingko episperm according to claim 1, it is characterized in that: in described step (4), extraction agent is sherwood oil or vinyl acetic monomer, and Solvent quantity is 1/3-1/2 mother liquor volume, extracts 2-3 time.
8. the Industrialized processing technique that extracts bilobalide from gingko episperm according to claim 1, it is characterized in that: described step (1) exosper replaces water soaking with 95% ethanol, the weight of 95% ethanol is 3-5 times of exosper, and stirring soak time is 3-6 hour.
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| CN2011104194017A CN103159779A (en) | 2011-12-15 | 2011-12-15 | Industrialization production technology for extracting bilobalide from Ginkgo testa |
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| CN2011104194017A CN103159779A (en) | 2011-12-15 | 2011-12-15 | Industrialization production technology for extracting bilobalide from Ginkgo testa |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102379296A (en) * | 2011-09-09 | 2012-03-21 | 北京农学院 | Novel use of ginkgolide C |
Citations (4)
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| CN1733768A (en) * | 2005-07-29 | 2006-02-15 | 四川恩威中医药研究开发有限公司 | Bilobalide extraction and purification process |
| CN101085780A (en) * | 2006-06-08 | 2007-12-12 | 天津天士力之骄药业有限公司 | Preparation method for ginkgolide |
| CN101134758A (en) * | 2007-10-15 | 2008-03-05 | 桂林市振达生物科技有限责任公司 | Method for extracting and separating bilobalide A, B, C, J and bilobalide monomer from ginkgo leaf |
| CN102174052A (en) * | 2011-03-23 | 2011-09-07 | 晨光生物科技集团天津有限公司 | Method for extracting and refining ginkgolide |
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2011
- 2011-12-15 CN CN2011104194017A patent/CN103159779A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1733768A (en) * | 2005-07-29 | 2006-02-15 | 四川恩威中医药研究开发有限公司 | Bilobalide extraction and purification process |
| CN101085780A (en) * | 2006-06-08 | 2007-12-12 | 天津天士力之骄药业有限公司 | Preparation method for ginkgolide |
| CN101134758A (en) * | 2007-10-15 | 2008-03-05 | 桂林市振达生物科技有限责任公司 | Method for extracting and separating bilobalide A, B, C, J and bilobalide monomer from ginkgo leaf |
| CN102174052A (en) * | 2011-03-23 | 2011-09-07 | 晨光生物科技集团天津有限公司 | Method for extracting and refining ginkgolide |
Non-Patent Citations (4)
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| 楼凤昌等: "银杏外种皮化学成分研究", 《中国药科大学学报》 * |
| 王成章等: "溶剂萃取银杏萜内酯的因子研究", 《天然产物研究与开发》 * |
| 邵胜荣: "银杏叶活性成分提取纯化、制剂工艺及质量研究", 《中国优秀硕士学位论文全文数据库（工程科技I辑）》 * |
| 韩金玉等: "银杏萜内酯提取与纯化技术", 《中草药》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102379296A (en) * | 2011-09-09 | 2012-03-21 | 北京农学院 | Novel use of ginkgolide C |
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Application publication date: 20130619 |