CN103159612A - Industrialization production technology for extracting ginkgolic acid from Ginkgo testa - Google Patents
Industrialization production technology for extracting ginkgolic acid from Ginkgo testa Download PDFInfo
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- CN103159612A CN103159612A CN2011104193851A CN201110419385A CN103159612A CN 103159612 A CN103159612 A CN 103159612A CN 2011104193851 A CN2011104193851 A CN 2011104193851A CN 201110419385 A CN201110419385 A CN 201110419385A CN 103159612 A CN103159612 A CN 103159612A
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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, 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.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 good using value is arranged; 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 ginkgoic acid is more, the 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, can't apply in industrialized production.
Summary of the invention
To extract ginkgoic acid 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 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 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 gets the ginkgoic acid of 60-70%;
(4) step (3) brown crystal is heated up after fully dissolving with alcoholic solution, the elimination insolubles is cooled to-5-20 ℃, separates out the light brown crystal, filters to get the ginkgoic acid of 90-95%;
(5) step (4) light brown crystal is added in weight 5-8 water doubly, regulate pH value to 8-10 with liquid caustic soda, fully after dissolving, add gac, heat up at whipped state, the insulation decolouring, elimination gac, mother liquor are cooled to 20-30 ℃, regulate pH value to 2-3 with acid solution, be cooled to-5-0 ℃, separate out white or off-white color solid, filter greater than 98% ginkgoic acid.
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), (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 ℃.
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 is regulated, and 70-80 ℃ of intensification temperature, soaking time are 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 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 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 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 (4) adopts alcoholic solution that the ginkgoic acid of crude product is washed, and can effectively improve the purity of ginkgoic acid; Step (5) adopts liquid caustic soda adjusting pH value to be alkalescence, and ginkgoic acid solubleness in basic solution than in water is low, when again being strongly-acid with acid solution adjusting pH value, 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 ℃ 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 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 in a large number, promptly extract ginkgoic acid 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 ginkgoic acid 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, and suction filtration gets 60% ginkgoic acid;
(4) step (3) brown crystal is heated up 50 ℃ fully after dissolving with ethanol, the elimination insolubles is cooled to 20 ℃, separates out the light brown crystal, filters to get 90% ginkgoic acid;
(5) step (4) light brown crystal being added in the water of 5 times of weight, is that 10% sodium hydroxide is regulated pH value to 8 with concentration, fully after dissolving, add 200 order gacs, gac weight is 2 ‰ of the rear total solution weight of sodium hydroxide adjusting, heats up 70 ℃ at whipped state, is incubated decolouring in 20 minutes, the elimination gac, mother liquor is cooled to 20 ℃, is that 10% hydrochloric acid is regulated pH value to 3 with concentration, is cooled to 0 ℃, separate out white or off-white color solid, filter greater than 98% ginkgoic acid.
Embodiment two
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 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, and suction filtration gets 65% ginkgoic acid;
(4) step (3) brown crystal is heated up 60 ℃ fully after dissolving with ethanol, the elimination insolubles is cooled to 13 ℃, separates out the light brown crystal, filters to get 93% ginkgoic acid;
(5) step (4) light brown crystal being added in the water of 6 times of weight, is that 20% sodium hydroxide is regulated pH value to 9 with concentration, fully after dissolving, add 200 order gacs, gac weight is 3 ‰ of the rear total solution weight of sodium hydroxide adjusting, heats up 75 ℃ at whipped state, is incubated decolouring in 25 minutes, the elimination gac, mother liquor is cooled to 25 ℃, is that 20% hydrochloric acid is regulated pH value to 2.5 with concentration, is cooled to-2 ℃, separate out white or off-white color solid, filter greater than 98% ginkgoic acid.
Embodiment three
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 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, and suction filtration gets 70% ginkgoic acid;
(4) step (3) brown crystal is heated up 70 ℃ fully after dissolving with ethanol, the elimination insolubles is cooled to-5 ℃, separates out the light brown crystal, filters to get 95% ginkgoic acid;
(5) step (4) light brown crystal being added in the water of 8 times of weight, is that 30% sodium hydroxide is regulated pH value to 10 with concentration, fully after dissolving, add 200 order gacs, gac weight is 4 ‰ of the rear total solution weight of sodium hydroxide adjusting, heats up 80 ℃ at whipped state, is incubated decolouring in 30 minutes, the elimination gac, mother liquor is cooled to 30 ℃, is that 30% hydrochloric acid is regulated pH value to 2 with concentration, is cooled to-5 ℃, separate out white or off-white color solid, filter greater than 98% ginkgoic acid.
Embodiment four
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 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, and suction filtration gets 70% ginkgoic acid;
(4) step (3) brown crystal is heated up 70 ℃ fully after dissolving with methyl alcohol, the elimination insolubles is cooled to-5 ℃, separates out the light brown crystal, filters to get 95% ginkgoic acid;
(5) step (4) light brown crystal being added in the water of 8 times of weight, is that 30% potassium hydroxide is regulated pH value to 10 with concentration, fully after dissolving, add 200 order gacs, gac weight is 4 ‰ of the rear total solution weight of potassium hydroxide adjusting, heats up 80 ℃ at whipped state, is incubated decolouring in 30 minutes, the elimination gac, mother liquor is cooled to 30 ℃, is that 30% oxalic acid is regulated pH value to 2 with concentration, is cooled to-5 ℃, separate out white or off-white color solid, filter greater than 98% ginkgoic acid.
But the ginkgoic acid of the every 1T gingko episperm of the present invention output 5-6Kg purity 98%, the industrialized utilization rate is higher.
Claims (8)
1. 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 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 gets the ginkgoic acid of 60-70%;
(4) step (3) brown crystal is heated up after fully dissolving with alcoholic solution, the elimination insolubles is cooled to-5-20 ℃, separates out the light brown crystal, filters to get the ginkgoic acid of 90-95%;
(5) step (4) light brown crystal is added in weight 5-8 water doubly, regulate pH value to 8-10 with liquid caustic soda, fully after dissolving, add gac, heat up at whipped state, the insulation decolouring, elimination gac, mother liquor are cooled to 20-30 ℃, regulate pH value to 2-3 with acid solution, be cooled to-5-0 ℃, separate out white or off-white color solid, filter greater than 98% ginkgoic acid.
2. the Industrialized processing technique that extracts ginkgoic acid 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 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, vinyl acetic monomer, oxalic acid, and acid solutions is 10-30%.
4. the Industrialized processing technique that extracts ginkgoic acid from gingko episperm according to claim 1, it is characterized in that: in described step (4), alcoholic solution is ethanol or methyl alcohol or both mixing solutionss, solvent temperature 50-70 ℃.
5. the Industrialized processing technique that extracts ginkgoic acid from gingko episperm according to claim 1, it is characterized in that: 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%.
6. the Industrialized processing technique that extracts 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 is regulated, 70-80 ℃ of intensification temperature, soaking time are 20-30 minute.
7. the Industrialized processing technique that extracts ginkgoic acid from gingko episperm according to claim 1, it is characterized in that: 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.
8. the Industrialized processing technique that extracts ginkgoic acid 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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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109053433A (en) * | 2018-07-27 | 2018-12-21 | 山东省分析测试中心 | A kind of method that combination prepares ginkgoic acid |
| CN112457427A (en) * | 2020-12-23 | 2021-03-09 | 湖北工程学院 | Method for extracting sulfated polysaccharide from ginkgo leaves and application thereof |
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| JP2005281155A (en) * | 2004-03-29 | 2005-10-13 | Japan Health Science Foundation | Cholesterol homeostasis-related gene transfer activity modifier via fxr activation |
| 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 |
-
2011
- 2011-12-15 CN CN201110419385.1A patent/CN103159612B/en not_active Expired - Fee Related
Patent Citations (3)
| 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 |
| 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 (2)
| Title |
|---|
| 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》 * |
| 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》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109053433A (en) * | 2018-07-27 | 2018-12-21 | 山东省分析测试中心 | A kind of method that combination prepares ginkgoic acid |
| CN109053433B (en) * | 2018-07-27 | 2021-03-19 | 山东省分析测试中心 | Combined preparation method of ginkgolic acid |
| CN112457427A (en) * | 2020-12-23 | 2021-03-09 | 湖北工程学院 | Method for extracting sulfated polysaccharide from ginkgo leaves and application thereof |
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| CN103159612B (en) | 2014-08-06 |
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