CN1763209A - Comprehensive utilization process for gingko episperm - Google Patents
Comprehensive utilization process for gingko episperm Download PDFInfo
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- CN1763209A CN1763209A CNA2005100945914A CN200510094591A CN1763209A CN 1763209 A CN1763209 A CN 1763209A CN A2005100945914 A CNA2005100945914 A CN A2005100945914A CN 200510094591 A CN200510094591 A CN 200510094591A CN 1763209 A CN1763209 A CN 1763209A
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- ethanol
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- gingko
- ginkgolic acid
- gingko episperm
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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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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Abstract
The comprehensive gingko outer seed coat utilizing process belongs to the field of gingko processing technology. Of the fresh gingko outer seed coat as material, the components capable of being fermented are water extracted as the fermentation culture medium and is fermented and extracted to produce alcohol, and the residue after water extraction is leached with 80 % concentration alcohol solution as the leaching solvent. The leached liquid is vacuum concentrated, separated and purified with macroporous resin LSA-21 and silica gel column successively to obtain gingko phenonic acid and similar matter in purity over 90 %. The present invention is significant in utilizing gingko resource and protecting ecologic environment.
Description
Technical field
A kind of technology that fully utilizes gingko episperm belongs to technical field of ginkgo processing.
Background technology
Ginkgo (ginkgo biloba L.) is a Ginkgoaceae Ginkgo plant, has another name called Gong Sunshu, maidenhair tree, is the endemic tree of China, also is a kind of in the world with a long history, precious resources of medicinal plant.Chemical ingredients in Ginkgo Leaf and the gingko and application have been carried out extensive studies both at home and abroad, the result shows that its leaf, fruit and exosper etc. all have medicinal exploitation to be worth, and many countries all are devoted to the ginkgo Products Development.China is ginkgo plantation big country, the gingko resource owning amount accounts for 70% of world's total amount, be Folium Ginkgo extract production and big export country, Jiangsu Province's ginkgo 2,000 ten thousand strains of now planting, build up 1.4 ten thousand hectares of production bases, produce 3600 tons of gingkoes per year, 4500 tons of dried leafiness, output ranks first in the whole country, and has the huge resources advantage of ginkgo industry development.
The fruit of ginkgo is commonly called as and is gingko, and having astringes the lung relievings asthma, and effects such as relieving cough and removing sputum have been developed to multiple nutrients food; Gingko episperm is commonly called as the gingko afterbirth, is the outer layer segment of ginkgo fruit, accounts for 70% of fruit weight, and utilization rate is low at present, does not still have the industrialization processing and utilization method of mature and reliable, generally is to be dropped as waste in the ginkgo producing region.According to estimates, China has 30,000 tons of fresh gingko episperms every year at least, if remove wherein about 60% moisture, dried gingko episperm has 1.2 ten thousand tons every year approximately.The long-term air storage of these gingko episperms, under the rainwater dipping, wherein contained phenolic acids toxic ingredient is entered the stream by water extraction, not only the place surrounding enviroment are stacked in influence, and the smell is awful, causes the wasting of resources, the more important thing is waters is on every side polluted, poison fishes and shrimps with poison, threaten people and animals' safety of drinking water, arrived must solution stage.If gingko episperm is not carried out harmless treatment, the industrialization of the ginkgo of just being far from being processing.Therefore, how carrying out the utilization of gingko episperm reasonable resources, administer environment, improve environment, is to promote ginkgo to process a urgent task in the further industrialization work.
After looking into newly, existing document all is at laboratory level gingko exocarp polysaccharide, flavones, phenolic acid to be tested, and finds no the report that closes the gingko episperm comprehensive utilization process.
Summary of the invention
The purpose of this invention is to provide a kind of technology of using biotechnology comprehensive utilization gingko episperm.With the yeast is that bacterial classification utilizes the fermentability composition fermentative production of ethanol in the gingko episperm water extract; Be solvent then with ethanol, extract gingko episperm water and carry the separating Ginkgo phenolic acids material that has bio-toxicity in the residue.The separating Ginkgo phenolic acids material can be developed as agricultural and go up widely used sterilant and sterilant.Carry out the comprehensive utilization of gingko episperm resource, improve its environmental pollution, reach the purpose that turns waste into wealth, promote ginkgo to process further industrialization work the ginkgo producing region.
Technical scheme of the present invention: for achieving the above object, the present invention is a raw material with the fresh gingko exosper, with fermentable composition water extract as the fermentation usefulness substratum, utilize active dry yeast (Mei Shan-Ma Li yeast company limited makes), utilize fermentability composition in the water extract, fermentative production of ethanol by fermentation.Be extraction solvent with 80% concentration ethanol then, the residue after lixiviate gingko episperm water is carried with gained extracting solution vacuum concentration, successively carries out separation and purification with macroporous resin LSA-21 and silicagel column, obtains the separating Ginkgo phenolic acids material of higher degree.Described technology is:
A, gingko episperm water extract fermentative production of ethanol
The first step: the after-ripening of ginkgo nut and decortication.
Fresh and the gingko episperm not any processing of process is difficult to directly peel off with kind benevolence, therefore with the ginkgo nut (solid substance 30～40% of fresh collection, moisture content 60～70%) puts into the after-ripening jar, by 1: 1.5 add the quality ratio, about soaking at room temperature 1～2 day, use mechanically peel again, get gingko episperm and ginkgo kernel.
Second step: homogenate.
Gingko episperm is mixed by 1: 0.5～1.5 mass ratioes with water, handle through tissue mashing machine or refiner.
The 3rd step: enzyme-added processing.
Feed liquid after refiner is handled is transferred pH4.5 with 10%HCl, and steam heating is warmed up to 50 ℃, presses the 4U/ml feed liquid and adds acidic cellulase, stirs enzymolysis 4～5h.
The 4th step: solid-liquid separation.
Solidliquid mixture after homogenate and the enzyme-added processing is handled through filter press or whizzer, made solid-liquid separation get milky filtrate A and filter residue B two portions.
The 5th step: fermentation.
Molasses are added in filtrate A sterilization back makes first sugared concentration be controlled at 15%, the inoculum size inoculation active dry yeast by 10%, and temperature: 30 ℃, fermentation time 40～50h.The shared volume fraction of the ethanol that is produced after the fermentation ends is 3%～5%.
The 6th step: fermented liquid distillation.
With the fermented liquid distillation, the control distillation temperature obtains the ethanol cut and is used for next stage extraction ginkgolic acid.
B, extraction and separation and purification ginkgolic acid
The first step: ethanol lixiviate filter residue B
Selecting 80% concentration ethanol is extraction solvent, and filter residue B and extraction solvent 80% concentration ethanol are pressed 1: 2～3 feed liquid mass ratio, and refluxing extraction is 3 times under 60 ℃ of conditions, each 3h, united extraction liquid filters, the filtrate evaporation concentration, control concentrated solution quality is 20% of a filter residue B quality.
Second step: macroporous resin LSA-21 chromatography.
Select for use the LSA-21 resin to carry out dynamic adsorption and desorb, the post specification is φ 20 * 150cm, and flow velocity is 0.3～0.5cm/min.Gingko episperm 80% concentration ethanol extract is filtered, vacuum concentration, again after dissolving with a small amount of dehydrated alcohol, upper prop, use twice column volume 20% concentration ethanol and twice column volume 40% concentration ethanol flush away impurity respectively, use twice column volume 80% concentration ethanol eluant solution again, the ethanol eluate of 80% concentration is concentrated into dried, promptly get thick ginkgolic acid.
The 3rd step: silica gel column chromatography.
For improving the purity of product ginkgolic acid, thick ginkgolic acid is further purified with silicagel column.Thick ginkgolic acid is added a small amount of sherwood oil dissolve again, last silicagel column (φ 20 * 150cm), and the petroleum ether-ethyl acetate-Glacial acetic acid of usefulness twice column volume (90: 10: 1, V/V) wash-out, flow velocity 0.3～0.5cm/min collects ginkgolic acid wash-out part.
The 4th step: concentrate drying.
Collect elutriant ginkgolic acid part, utilize the vacuum concentration instrument to concentrate, reclaim organic solvent.The dry ginkgolic acid dry powder that gets of concentrated solution, purity is greater than 90%.
The measuring method of ginkgolic acid: fluorescence spectrophotometry ginkgolic acid.At excitation wavelength lambda ex=345nm, under the condition of emission wavelength lambda em=420nm, as blank, measure ginkgolic acid standard operation fluorescence intensity of solution with methyl alcohol, corresponding concentration is mapped the drawing standard curve with fluorescence intensity.The fluorescence intensity of total ginkgolic acid in the working sample solution under identical condition is again by its content of regression equation calculation.
Beneficial effect of the present invention: raw material gingko episperm of the present invention belongs to waste, and is in liberal supply; Processing back purpose product ethanol and separating Ginkgo phenolic acids material have stable selling market.The separating Ginkgo phenolic acids material can be developed as agricultural and go up widely used sterilant and sterilant.The comprehensive utilization of accelerating exploitation and enforcement gingko episperm has tangible economic benefit, environmental benefit and social benefit.
Eliminate the pollution of gingko episperm, the safety of protection people and animals' Drinking Water and water fish shrimp to processing region surrounding enviroment.
Turn waste into wealth, prevent the waste of resource, promote the further development of ginkgo plantation and processing industry, the government and the people that plant the region for ginkgo increase income.
Gingko episperm prepares biological pesticide, can increase new biological pesticide kind for the domestic market, improves the nuisanceless quality of green vegetables, fruit etc.
The present invention to the comprehensive utilization gingko resource, preserving the ecological environment all has very important meaning.
Description of drawings
Fig. 1 fully utilizes the process schematic representation of gingko episperm.
Embodiment
Embodiment 1
1 ton of fresh ginkgo nut immerses in 1.5 tons of water, soaking at room temperature 24 hours, and the machinery decortication gets 0.30 ton of gingko, 0.70 ton of exosper.Exosper is mixed by 1: 1 mass ratio with water, handle through refiner, transfer pH4.5 with 10%HCl, steam heating is warmed up to 50 ℃, presses the 4U/ml feed liquid and adds acidic cellulase, stirs enzymolysis 4～5h.Solidliquid mixture after homogenate and the enzyme-added processing is handled through filter press or whizzer, made solid-liquid separation get 0.50 ton of 0.9 ton of milky filtrate and filter residue.Molasses are added in filtrate sterilization back makes first saccharic amount concentration be controlled at 15%, the inoculum size inoculation active dry yeast by 10%, and temperature: 30 ℃, fermentation time 40～50h.The shared volume fraction of the ethanol that is produced after the fermentation ends is 3%～5%.Fermented liquid is concentrated distillation, and gained ethanol is used for next stage extraction ginkgolic acid.
Selecting 80% ethanol is extraction solvent, and filter residue and 80% concentration ethanol are pressed 1: 2～3 feed liquid mass ratio, and refluxing extraction is 3 times under 60 ℃ of conditions, each 3h, and united extraction liquid filters, the filtrate evaporation concentration, control concentrated solution quality is 20% of a filter residue B quality.Select for use the LSA-21 resin to adsorb and desorb, the post specification is φ 20 * 150cm, and flow velocity is 0.3～0.5cm/min.Gingko episperm 80% concentration ethanol extract is filtered, vacuum concentration, after dissolving again with a small amount of dehydrated alcohol, upper prop is used 20%, 40%, 80% concentration ethanol eluant solution of each twice column volume respectively.The ethanol eluate of 80% concentration is concentrated into dried, promptly gets thick ginkgolic acid, purity is greater than 60%.For improving the purity of product ginkgolic acid, thick ginkgolic acid is further purified with silicagel column.Thick ginkgolic acid is added a small amount of sherwood oil to be dissolved again, (φ 20 * 150cm) for last silicagel column, with the petroleum ether-ethyl acetate-Glacial acetic acid of twice column volume (90: 10: 1, V/V) wash-out, flow velocity is 0.3～0.5cm/min, collect elutriant ginkgolic acid part, utilize the vacuum concentration instrument to concentrate, reclaim organic solvent.The dry ginkgolic acid dry powder 8～12kg that gets of concentrated solution, purity is greater than 90%.
Claims (1)
1, a kind of technology that fully utilizes gingko episperm, it is characterized in that with the fresh gingko exosper be raw material, fermentable composition water is extracted substratum as fermentation usefulness, utilize active dry yeast to utilize fermentability composition in the water extract, fermentative production of ethanol by fermentation; Be extraction solvent with 80% concentration ethanol then, the residue after lixiviate gingko episperm water is carried with gained extracting solution vacuum concentration, successively carries out separation and purification with macroporous resin LSA-21 and silicagel column, obtains highly purified separating Ginkgo phenolic acids material, and described technology is:
A, gingko episperm water extract fermentative production of ethanol
(1) after-ripening of ginkgo nut and decortication: the ginkgo nut of fresh collection is put into the after-ripening jar, by 1: 1.5 add the quality ratio, soaking at room temperature 1～2 day is used mechanically peel again, gingko episperm and ginkgo kernel;
(2) homogenate: gingko episperm is mixed by 1: 0.5～1.5 mass ratioes with water, through tissue mashing machine or refiner homogenate;
(3) enzymolysis: the feed liquid after the homogenate, transfer pH4.5 with 10%HCl, steam heating is warmed up to 50 ℃, presses the 4U/ml feed liquid and adds acidic cellulase, stirs enzymolysis 4～5h;
(4) solid-liquid separation: the solidliquid mixture behind the enzymolysis is handled through filter press or whizzer, made solid-liquid separation get milky filtrate A and filter residue B two portions;
(5) fermentation: molasses are added in filtrate A sterilization back makes first saccharic amount concentration be controlled at 15%, the inoculum size inoculation active dry yeast by 10%, and leavening temperature: 30 ℃, fermentation time 40～50h, the shared volume fraction of the ethanol that produces after the fermentation ends is 3%～5%;
(6) fermented liquid distillation: with the fermented liquid distillation, the control distillation temperature obtains the ethanol cut and is used for next stage extraction ginkgolic acid;
B, extraction and separation and purification ginkgolic acid
(7) ethanol lixiviate filter residue B: selecting 80% concentration ethanol is extraction solvent, filter residue B and extraction solvent 80% concentration ethanol are pressed 1: 2～3 feed liquid mass ratio, refluxing extraction is 3 times under 60 ℃ of conditions, each 3h, united extraction liquid, filter, the filtrate evaporation concentration, control concentrated solution quality is 20% of a filter residue B quality;
(8) macroporous resin LSA-21 chromatography: select for use the LSA-21 resin to adsorb and desorb, the post specification is φ 20 * 150cm, flow velocity is 0.3～0.5cm/min, gingko episperm 80% concentration ethanol extract is filtered, vacuum concentration, again after dissolving with a small amount of dehydrated alcohol, upper prop, use twice column volume 20% concentration ethanol and twice column volume 40% concentration ethanol flush away impurity respectively, use twice column volume 80% concentration ethanol eluant solution again, the ethanol eluate of 80% concentration is concentrated into dried, promptly gets thick ginkgolic acid;
(9) silica gel column chromatography: thick ginkgolic acid is added a small amount of sherwood oil dissolve again, last silicagel column φ 20 * 150cm is with the petroleum ether-ethyl acetate-Glacial acetic acid of twice column volume, volume ratio is 90: 10: 1, wash-out, flow velocity 0.3～0.5cm/min collects ginkgolic acid wash-out part;
(10) concentrate drying: collect elutriant ginkgolic acid part, utilize the vacuum concentration instrument to concentrate, reclaim organic solvent, the dry ginkgolic acid dry powder that gets of concentrated solution, purity is greater than 90%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100945914A CN1321189C (en) | 2005-09-26 | 2005-09-26 | Comprehensive utilization process for gingko episperm |
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| CNB2005100945914A CN1321189C (en) | 2005-09-26 | 2005-09-26 | Comprehensive utilization process for gingko episperm |
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| CN1321189C CN1321189C (en) | 2007-06-13 |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101156703B (en) * | 2007-11-16 | 2010-06-02 | 江南大学 | A method for preparing water-solubility ginkgo powder |
| CN102349919A (en) * | 2011-08-18 | 2012-02-15 | 王青 | Application of gingkolic acid in preparation of external preparation for treating osmidrosis |
| CN101531590B (en) * | 2009-04-21 | 2012-04-18 | 福州大学 | Ginkgoic acid preparation method using macroporous adsorption resin |
| CN102846677A (en) * | 2012-08-14 | 2013-01-02 | 王青 | Use of ginkgolic acids in preparation of external preparation for treating cutaneous tumors |
| 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 |
| CN106360727A (en) * | 2016-11-22 | 2017-02-01 | 江南大学 | Comprehensive utilization method for plants |
| CN106538521A (en) * | 2016-10-11 | 2017-03-29 | 常州市鼎日环保科技有限公司 | A kind of preparation method of degradable noresidue fruits and vegetables insecticidal dust |
| CN106578403A (en) * | 2016-12-07 | 2017-04-26 | 江南大学 | Comprehensive utilization method for perilla seed meal |
| CN106636214A (en) * | 2016-09-21 | 2017-05-10 | 郑华 | Ginkgo biloba exocarp fermentation liquid as well as preparation method and application thereof |
| CN106832045A (en) * | 2015-12-02 | 2017-06-13 | 中国科学院大连化学物理研究所 | A kind of method that gingko episperm extracts pectin and phenolic acid compound simultaneously |
| CN109287665A (en) * | 2018-09-25 | 2019-02-01 | 临沂大学 | A kind of ginkgolic acid-avermectin composite insecticide and preparation method thereof |
| CN116899271A (en) * | 2023-09-14 | 2023-10-20 | 焱农(济南)生物科技有限公司 | Preparation method of high-content ginkgolic acid biological pesticide raw material and prepared raw material |
| CN117814265A (en) * | 2024-03-01 | 2024-04-05 | 临沂大学 | Method for fermenting ginkgo exocarp by microorganisms and application thereof |
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| JP2003061612A (en) * | 2001-08-29 | 2003-03-04 | Amano:Kk | Fermented liquid for health food and method for producing the same |
| CN1160447C (en) * | 2001-09-07 | 2004-08-04 | 李改成 | Ginkgo vinegar and its preparation method |
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- 2005-09-26 CN CNB2005100945914A patent/CN1321189C/en not_active Expired - Fee Related
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101156703B (en) * | 2007-11-16 | 2010-06-02 | 江南大学 | A method for preparing water-solubility ginkgo powder |
| CN101531590B (en) * | 2009-04-21 | 2012-04-18 | 福州大学 | Ginkgoic acid preparation method using macroporous adsorption resin |
| CN102349919A (en) * | 2011-08-18 | 2012-02-15 | 王青 | Application of gingkolic acid in preparation of external preparation for treating osmidrosis |
| CN102349919B (en) * | 2011-08-18 | 2013-08-14 | 王青 | Application of gingkolic acid in preparation of external preparation for treating osmidrosis |
| CN102846677A (en) * | 2012-08-14 | 2013-01-02 | 王青 | Use of ginkgolic acids in preparation of external preparation for treating cutaneous tumors |
| CN106832045A (en) * | 2015-12-02 | 2017-06-13 | 中国科学院大连化学物理研究所 | A kind of method that gingko episperm extracts pectin and phenolic acid compound simultaneously |
| CN106832045B (en) * | 2015-12-02 | 2018-12-14 | 中国科学院大连化学物理研究所 | A kind of method that gingko episperm extracts pectin and phenolic acid compound simultaneously |
| 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 |
| 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 |
| CN106636214A (en) * | 2016-09-21 | 2017-05-10 | 郑华 | Ginkgo biloba exocarp fermentation liquid as well as preparation method and application thereof |
| CN106538521A (en) * | 2016-10-11 | 2017-03-29 | 常州市鼎日环保科技有限公司 | A kind of preparation method of degradable noresidue fruits and vegetables insecticidal dust |
| CN106360727A (en) * | 2016-11-22 | 2017-02-01 | 江南大学 | Comprehensive utilization method for plants |
| CN106360727B (en) * | 2016-11-22 | 2023-06-27 | 江南大学 | Comprehensive utilization method of plants |
| CN106578403A (en) * | 2016-12-07 | 2017-04-26 | 江南大学 | Comprehensive utilization method for perilla seed meal |
| CN109287665A (en) * | 2018-09-25 | 2019-02-01 | 临沂大学 | A kind of ginkgolic acid-avermectin composite insecticide and preparation method thereof |
| CN109287665B (en) * | 2018-09-25 | 2021-03-02 | 临沂大学 | Ginkgolic acid-abamectin composite pesticide and preparation method thereof |
| CN116899271A (en) * | 2023-09-14 | 2023-10-20 | 焱农(济南)生物科技有限公司 | Preparation method of high-content ginkgolic acid biological pesticide raw material and prepared raw material |
| CN116899271B (en) * | 2023-09-14 | 2023-12-12 | 焱农(济南)生物科技有限公司 | Preparation method of high-content ginkgolic acid biological pesticide raw material and prepared raw material |
| CN117814265A (en) * | 2024-03-01 | 2024-04-05 | 临沂大学 | Method for fermenting ginkgo exocarp by microorganisms and application thereof |
| CN117814265B (en) * | 2024-03-01 | 2024-05-17 | 临沂大学 | Method for fermenting ginkgo exocarp by microorganisms and application thereof |
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