CN103159612B - Industrialization production technology for extracting ginkgolic acid from Ginkgo testa - Google Patents
Industrialization production technology for extracting ginkgolic acid from Ginkgo testa Download PDFInfo
- Publication number
- CN103159612B CN103159612B CN201110419385.1A CN201110419385A CN103159612B CN 103159612 B CN103159612 B CN 103159612B CN 201110419385 A CN201110419385 A CN 201110419385A CN 103159612 B CN103159612 B CN 103159612B
- Authority
- CN
- China
- Prior art keywords
- acid
- extracting
- solution
- ginkgoic
- ginkgoic acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention relates to an industrialization production technology for extracting ginkgolic acid 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; crystallizing, recrystallizing, and decolorizing by alkali liquor and acid precipitation; and further purifying the ginkgolic acid. The invention employs acid solution to regulate the pH value of the solution containing ginkgolic acid, and precipitates the ginkgolic acid 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 ginkgolic acid 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 ginkgoic acid 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, American-European have all carried out deep development to it, in succession develop multiple medicine, and healthcare products and makeup, make a profit considerable.China also payes attention to all the more on to the comprehensive utilization of ginkgo nut, Ginkgo Leaf.But, account for the gingko episperm of the most of weight of ginkgo fruit generally when waste abandons, fail to be fully used, simultaneously to environment.
After deliberation, in gingko episperm, the contained substances content such as ginkgoic acid, bilobalide is the contained 2-3 of ginkgo nut or Ginkgo Leaf times, has to extract to be worth.The effects such as that ginkgoic acid has is anti-oxidant, anti-inflammatory, antitumor, antianaphylaxis, antibacterial, prevention and elimination of disease and pests, food, makeup, biological pesticide and medical aspect have good using value; Its structure is:
The extractive technique of gingko episperm is all had to relevant report both at home and abroad.At present, conventional extracting method 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 ginkgoic acid is more, said extracted method is only suitable for extracting for the ginkgoic acid 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, cannot in industrialized production, apply.
Summary of the invention
In prior art, to extract ginkgoic acid in gingko episperm and cannot be applicable to the drawback in industrialized production in order to solve, the invention provides a kind of technique simple, easy to operate, production cost is low, extraction yield is high, extraction accuracy is high, can meet the Industrialized processing technique that extracts ginkgoic acid from gingko episperm of industrialized production requirement.
The technical solution used in the present invention is: a kind of Industrialized processing technique that extracts ginkgoic acid from gingko episperm, is characterized in that comprising the following steps:
(1) gingko episperm after cleaning is ground to carefully, crosses 30-80 order, add in weight 5-10 water doubly, stir and soak 5-12 hour;
(2) the mixed solution centrifugation after soaking is removed slag, filtrate is pumped in concentrating pan, vacuum fractionation is concentrated;
(3) after concentrated, in solution, add acid solution and regulate pH value to 2-3, be cooled to-5-10 DEG C, separate out brown crystal, suction filtration obtains the ginkgoic acid of 60-70%;
(4) after step (3) brown crystal is heated up and fully dissolved with alcoholic solution, elimination insolubles, is cooled to-5-20 DEG C, separates out light brown crystal, filters to obtain the ginkgoic acid of 90-95%;
(5) step (4) light brown crystal is added in weight 5-8 water doubly, to 8-10, after fully dissolving, add gac with liquid caustic soda adjusting pH value, heat up at whipped state, insulation decolouring, elimination gac, mother liquor is cooled to 20-30 DEG C, with acid solution regulate pH value to 2-3, be cooled to-5-0 DEG C, separate out white or off-white color solid, filter to such an extent that be greater than 98% ginkgoic acid.
Described step (2) vacuum fractionation is concentrated, the component of fractionation 48-70 DEG C under the vacuum tightness of 0.08-0.09Mpa.
In described step (3), (5), 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), alcoholic solution is ethanol or methyl alcohol or both mixing solutionss, solvent temperature 50-70 DEG C.
In described step (5), liquid caustic soda is sodium hydroxide or potassium hydroxide or both mixing solutionss, and liquid caustic soda concentration is 10-30%.
In described step (5), gac is 200 orders, and gac weight is the 2-4 ‰ of total solution weight after liquid caustic soda regulates, intensification temperature 70-80 DEG C, and soaking time is 20-30 minute.
In described step (6), 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 doubly, stirring soak time is 3-6 hour to the 3-5 that the weight of 95% ethanol is exosper.
Compared with prior art, the present invention has the following advantages:
1, the solution that contains ginkgoic acid in step (3), (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 ginkgoic acid, realize a large amount of separation of ginkgoic acid, compare in biological extraction technology factors such as equipment and environmental requirement, extracted amount and costs, have easy to operately, technique is simple, low to equipment and environmental requirement, extraction yield is high, advantage with low cost;
2, step (4) adopts alcoholic solution to wash the ginkgoic acid of crude product, can effectively improve the purity of ginkgoic acid; Step (5) adopts liquid caustic soda to regulate pH value to be alkalescence, and ginkgoic acid solubleness in basic solution than in water is low, in the time again regulating pH value to be strongly-acid with acid solution, has improved the eduction rate of ginkgoic acid; Coordinate activated carbon insulation decolouring, further improve the purity of final ginkgoic acid;
3, in step (2), vacuum fractionation is concentrated, the component of fractionation 48-70 DEG C 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, there is the effect of good prevention and elimination of disease and pests, there is bacteriostasis, preservation effect simultaneously, can directly be used as desinsection, antiseptic-germicide, preservation agent, further improve 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 conventional raw material of suitability for industrialized production, and use cost is low, can repeat to reclaim to use.
The present invention utilizes acid solution to regulate the pH value of composition containing ginkgo acid solution, by common-ion effcet, ginkgoic acid 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 from ginkgo exterior skin, in a large number, promptly extract ginkgoic acid, be applicable to the requirement of industrialized production.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment mono-
From gingko episperm, extract an Industrialized processing technique for ginkgoic acid, it is characterized in that comprising the following steps:
(1) gingko episperm after cleaning is ground to carefully, crosses 30 orders, add in the water of 5 times of weight, stir and soak 5 hours;
(2) the mixed solution centrifugation after soaking is removed slag, filtrate is pumped in concentrating pan, under the vacuum tightness of 0.08Mpa, vacuum fractionation goes out the component of 48 DEG C, and concentrated;
(3) after concentrated, in solution, adding concentration is that 10% hydrochloric acid regulates pH value to 3, is cooled to 10 DEG C, separates out brown crystal, and suction filtration obtains 60% ginkgoic acid;
(4) after step (3) brown crystal is heated up 50 DEG C and fully dissolved with ethanol, elimination insolubles, is cooled to 20 DEG C, separates out light brown crystal, filters to obtain 90% ginkgoic acid;
(5) step (4) light brown crystal being added in the water of 5 times of weight, is that 10% sodium hydroxide regulates pH value to 8 by concentration, after fully dissolving, add 200 order gacs, gac weight is 2 ‰ of the rear total solution weight of sodium hydroxide adjusting, heats up 70 DEG C at whipped state, is incubated decolouring in 20 minutes, elimination gac, mother liquor is cooled to 20 DEG C, is that 10% hydrochloric acid regulates pH value to 3 by concentration, is cooled to 0 DEG C, separate out white or off-white color solid, filter to such an extent that be greater than 98% ginkgoic acid.
Embodiment bis-
From gingko episperm, extract an Industrialized processing technique for ginkgoic acid, it is characterized in that comprising the following steps:
(1) gingko episperm after cleaning is ground to carefully, crosses 60 orders, add in the water of 8 times of weight, stir and soak 8 hours;
(2) the mixed solution centrifugation after soaking is removed slag, filtrate is pumped in concentrating pan, under the vacuum tightness of 0.085Mpa, vacuum fractionation goes out the component of 60 DEG C, and concentrated;
(3) after concentrated, in solution, adding concentration is that 20% hydrochloric acid regulates pH value to 2.5, is cooled to 2 DEG C, separates out brown crystal, and suction filtration obtains 65% ginkgoic acid;
(4) after step (3) brown crystal is heated up 60 DEG C and fully dissolved with ethanol, elimination insolubles, is cooled to 13 DEG C, separates out light brown crystal, filters to obtain 93% ginkgoic acid;
(5) step (4) light brown crystal being added in the water of 6 times of weight, is that 20% sodium hydroxide regulates pH value to 9 by concentration, after fully dissolving, add 200 order gacs, gac weight is 3 ‰ of the rear total solution weight of sodium hydroxide adjusting, heats up 75 DEG C at whipped state, is incubated decolouring in 25 minutes, elimination gac, mother liquor is cooled to 25 DEG C, is that 20% hydrochloric acid regulates pH value to 2.5 by concentration, is cooled to-2 DEG C, separate out white or off-white color solid, filter to such an extent that be greater than 98% ginkgoic acid.
Embodiment tri-
From gingko episperm, extract an Industrialized processing technique for ginkgoic acid, it is characterized in that comprising the following steps:
(1) gingko episperm after cleaning is ground to carefully, crosses 80 orders, add in the water of 10 times of weight, stir and soak 12 hours;
(2) the mixed solution centrifugation after soaking is removed slag, filtrate is pumped in concentrating pan, under the vacuum tightness of 0.09Mpa, vacuum fractionation goes out the component of 70 DEG C, and concentrated;
(3) after concentrated, in solution, adding concentration is that 30% hydrochloric acid regulates pH value to 2, is cooled to-5 DEG C, separates out brown crystal, and suction filtration obtains 70% ginkgoic acid;
(4) after step (3) brown crystal is heated up 70 DEG C and fully dissolved with ethanol, elimination insolubles, is cooled to-5 DEG C, separates out light brown crystal, filters to obtain 95% ginkgoic acid;
(5) step (4) light brown crystal being added in the water of 8 times of weight, is that 30% sodium hydroxide regulates pH value to 10 by concentration, after fully dissolving, add 200 order gacs, gac weight is 4 ‰ of the rear total solution weight of sodium hydroxide adjusting, heats up 80 DEG C at whipped state, is incubated decolouring in 30 minutes, elimination gac, mother liquor is cooled to 30 DEG C, is that 30% hydrochloric acid regulates pH value to 2 by concentration, is cooled to-5 DEG C, separate out white or off-white color solid, filter to such an extent that be greater than 98% ginkgoic acid.
Embodiment tetra-
From gingko episperm, extract an Industrialized processing technique for ginkgoic acid, it is characterized in that comprising the following steps:
(1) gingko episperm after cleaning is ground to carefully, crosses 80 orders, add in 95% ethanol of 5 times of weight, stir and soak 6 hours;
(2) the mixed solution centrifugation after soaking is removed slag, filtrate is pumped in concentrating pan, under the vacuum tightness of 0.09Mpa, vacuum fractionation goes out the component of 70 DEG C, and concentrated;
(3) after concentrated, in solution, adding concentration is that 30% oxalic acid regulates pH value to 2, is cooled to-5 DEG C, separates out brown crystal, and suction filtration obtains 70% ginkgoic acid;
(4) after step (3) brown crystal is heated up 70 DEG C and fully dissolved with methyl alcohol, elimination insolubles, is cooled to-5 DEG C, separates out light brown crystal, filters to obtain 95% ginkgoic acid;
(5) step (4) light brown crystal being added in the water of 8 times of weight, is that 30% potassium hydroxide regulates pH value to 10 by concentration, after fully dissolving, add 200 order gacs, gac weight is 4 ‰ of the rear total solution weight of potassium hydroxide adjusting, heats up 80 DEG C at whipped state, is incubated decolouring in 30 minutes, elimination gac, mother liquor is cooled to 30 DEG C, is that 30% oxalic acid regulates pH value to 2 by concentration, is cooled to-5 DEG C, separate out white or off-white color solid, filter to such an extent that be greater than 98% ginkgoic acid.
The every 1T gingko episperm of the present invention can output 5-6Kg purity 98% ginkgoic acid, industrialized utilization rate is higher.
Claims (7)
1. a production method of extracting ginkgoic acid from gingko episperm, is characterized in that comprising the following steps:
(1) gingko episperm after cleaning is ground to carefully, crosses 30-80 order, add in weight 5-10 water doubly, stir and soak 5-12 hour;
(2) the mixed solution centrifugation after soaking is removed slag, filtrate is pumped in concentrating pan, vacuum fractionation is concentrated;
(3) after concentrated, in solution, add acid solution and regulate pH value to 2-3, be cooled to-5-10 DEG C, separate out brown crystal, suction filtration obtains the ginkgoic acid of 60-70%;
(4) after step (3) brown crystal is heated up and fully dissolved with alcoholic solution, elimination insolubles, is cooled to-5-20 DEG C, separates out light brown crystal, filters to obtain the ginkgoic acid of 90-95%;
(5) step (4) light brown crystal is added in weight 5-8 water doubly, to 8-10, after fully dissolving, add gac by liquid caustic soda adjusting pH value, heat up at whipped state, insulation decolouring, elimination gac, mother liquor is cooled to 20-30 DEG C, regulate pH value to 2-3 with acid solution, be cooled to-5-0 DEG C, separate out white or off-white color solid, filter to such an extent that be greater than 98% ginkgoic acid.
2. the production method of extracting ginkgoic acid from gingko episperm according to claim 1, is characterized in that: described step (2) vacuum fractionation is concentrated, the component of fractionation 48-70 DEG C under the vacuum tightness of 0.08-0.09MPa.
3. the production method of extracting ginkgoic acid from gingko episperm according to claim 1, it is characterized in that: in described step (3), (5), acid solution is any one or two or more mixing solutions in hydrochloric acid, phosphoric acid, sulfuric acid, oxalic acid, and acid solutions is 10-30%.
4. the production method of extracting ginkgoic acid from gingko episperm according to claim 1, is characterized in that: in described step (4), alcoholic solution is ethanol or methyl alcohol or both mixing solutionss, solvent temperature 50-70 DEG C.
5. the production method of extracting ginkgoic acid from gingko episperm according to claim 1, is characterized in that: in described step (5), liquid caustic soda is sodium hydroxide, and liquid caustic soda concentration is 10-30%.
6. the production method of extracting ginkgoic acid from gingko episperm according to claim 1, it is characterized in that: in described step (5), gac is 200 orders, gac weight is the 2-4 ‰ of total solution weight after liquid caustic soda regulates, intensification temperature 70-80 DEG C, and soaking time is 20-30 minute.
7. the production method of extracting ginkgoic acid from gingko episperm according to claim 1, it is characterized in that: described step (1) exosper 95% ethanol replaces water soaking, the weight of 95% ethanol is 3-5 times of exosper, and stirring soak time is 3-6 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110419385.1A CN103159612B (en) | 2011-12-15 | 2011-12-15 | Industrialization production technology for extracting ginkgolic acid from Ginkgo testa |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110419385.1A CN103159612B (en) | 2011-12-15 | 2011-12-15 | Industrialization production technology for extracting ginkgolic acid from Ginkgo testa |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103159612A CN103159612A (en) | 2013-06-19 |
| CN103159612B true CN103159612B (en) | 2014-08-06 |
Family
ID=48583181
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110419385.1A Expired - Fee Related CN103159612B (en) | 2011-12-15 | 2011-12-15 | Industrialization production technology for extracting ginkgolic acid from Ginkgo testa |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103159612B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109053433B (en) * | 2018-07-27 | 2021-03-19 | 山东省分析测试中心 | Combined preparation method of ginkgolic acid |
| CN112457427B (en) * | 2020-12-23 | 2022-06-07 | 湖北工程学院 | Method for extracting sulfated polysaccharide from ginkgo leaves and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1806544A (en) * | 2006-02-21 | 2006-07-26 | 复旦大学 | Use of ginkgoic acid in preparation of biological pesticide for killing Oncomelania snail and preventing schistosomiasis |
| CN1871907A (en) * | 2006-06-23 | 2006-12-06 | 江苏大学 | Use of ginkgoic acid in use for killing Oncomelania snail distilled from outer seed coat of gingkgo |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005281155A (en) * | 2004-03-29 | 2005-10-13 | Japan Health Science Foundation | Cholesterol homeostasis-related gene transfer activity modifier via fxr activation |
-
2011
- 2011-12-15 CN CN201110419385.1A patent/CN103159612B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1806544A (en) * | 2006-02-21 | 2006-07-26 | 复旦大学 | Use of ginkgoic acid in preparation of biological pesticide for killing Oncomelania snail and preventing schistosomiasis |
| CN1871907A (en) * | 2006-06-23 | 2006-12-06 | 江苏大学 | Use of ginkgoic acid in use for killing Oncomelania snail distilled from outer seed coat of gingkgo |
Non-Patent Citations (5)
| Title |
|---|
| JP特开2005-281155A 2005.10.13 |
| Preparative isolation and dual column high-performance liquid chromatography of ginkgolic acids from Ginkgo biloba;Teris A. van Beek et al.;《Journal of Chromatography A》;20011231;第930卷;第109–117页 * |
| Teris A. van Beek et al..Preparative isolation and dual column high-performance liquid chromatography of ginkgolic acids from Ginkgo biloba.《Journal of Chromatography A》.2001,第930卷第109–117页. |
| 不同工艺提取银杏外种皮中银杏酸及含量的测定;王志强 等;《现代农业科技》;20091220(第24期);第326和328页 * |
| 王志强 等.不同工艺提取银杏外种皮中银杏酸及含量的测定.《现代农业科技》.2009,(第24期),第326和328页. |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103159612A (en) | 2013-06-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102048885B (en) | Extraction process for lychee seed saponin | |
| CN103086889B (en) | A kind of method of enzyme catalysis activation leaf of Flos Lonicerae chlorogenic acid extracting | |
| CN102229628B (en) | Method for extracting persimmon tannin from persimmons | |
| CN102994350B (en) | Preparation method of tartary buckwheat wine with function of reducing blood fat | |
| CN103263514A (en) | Method for extracting flavones, low-molecule pectin and cellulose from orange peels in combined way | |
| CN103432562A (en) | Method for extracting fresh ginger polyphenol from fresh ginger | |
| CN104593441A (en) | Method for simultaneously extracting volatile oil, polysaccharides and amino acids from tricholoma matsutake | |
| CN107118253B (en) | The preparation method of Tea Saponin | |
| CN102643315A (en) | Method for purifying phlorizin from apple velamen | |
| CN103739638B (en) | A kind of method of fermentable purifying tea saponin | |
| CN105399795B (en) | Method for extracting astragaloside from radix astragali | |
| CN103159612B (en) | Industrialization production technology for extracting ginkgolic acid from Ginkgo testa | |
| CN102492666A (en) | Enzyme preparation, application and method for extracting pueraria flavonid by enzyme preparation thereof | |
| CN101759731B (en) | Extraction method of linseed gum and secoisolariciresin-ol diglucoside | |
| CN105943568A (en) | Acorn polyphenol extracting and purifying method | |
| CN102432575B (en) | Method for extracting high-purity hesperetin from immature bitter orange | |
| CN104311616A (en) | Method for extracting high-purity esculine and fraxin from Cortex Fraxini | |
| CN103159619A (en) | Industrialization production technology for extracting ginkgolic acid and bilobalide from Ginkgo testa | |
| CN104231011B (en) | Preparation method of verbascoside | |
| CN105412167A (en) | Method for extracting and separating ginkgo flavone and ginkgolide from ginkgo leaves | |
| CN104945532A (en) | Preparing method for gynura divaricata polysaccharide | |
| CN102051393A (en) | Method for extracting camptothecin and 9-methoxyl camptothecin from root-bark of pittosporumlike nothapodytes | |
| CN103740778B (en) | The method of dihydroquercetin and rhamnosyl is extracted from Folium Engelhardia roxburghina | |
| CN107473970A (en) | It is a kind of to extract the linolenic method of high-purity alpha by raw material of linseed | |
| CN104163877B (en) | The preparation method of chondroitin sulfate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140806 Termination date: 20191215 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |