CN104435016A - Preparation process of ginkgo leaf extract - Google Patents
Preparation process of ginkgo leaf extract Download PDFInfo
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- CN104435016A CN104435016A CN201310440422.6A CN201310440422A CN104435016A CN 104435016 A CN104435016 A CN 104435016A CN 201310440422 A CN201310440422 A CN 201310440422A CN 104435016 A CN104435016 A CN 104435016A
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- folium ginkgo
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- ginkgo extract
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/16—Ginkgophyta, e.g. Ginkgoaceae (Ginkgo family)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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Abstract
The invention relates to a preparation process of a ginkgo leaf extract, belonging to the field of refining of natural plant extracts. The preparation process of the ginkgo leaf extract comprises the following steps: (1) extracting, namely removing impurities in ginkgo leaves, extracting the whole ginkgo leaves by taking ethanol as an extracting agent for three times in each of the three rounds, wherein the extracts obtained in the later two times of the first round are mixed together to be used in the first time of the second round, new solvents are used in the second time and third time of the second round, and extracts obtained in the later two times of the second round are mixed to be used in the first time of the third round; (2) concentrating, namely concentrating the extracts obtained in the first time of each round at reduced pressure until the extracts do not contain ethanol, and adding water to dilute the concentrated extracts; (3) precipitating, namely adding an enzymic preparation into the diluted extracts to stand and precipitate at room temperature; (4) centrifuging; (5) treating with a resin: (6) concentrating to obtain the desorbed concentrate of the ginkgo leaf extract; and (7) spray-drying and sterilizing to obtain the low-acid powdery ginkgo leaf extract. The preparation process of the ginkgo leaf extract is simple and is low in cost, and the use amount of solvents is reduced greatly.
Description
Technical field
The present invention relates to a kind of preparation technology of Folium Ginkgo extract, belong to natural plant extracts field of refinement.
Background technology
China is the original producton location of Semen Ginkgo, is again the main producing region of world Semen Ginkgo, and current China gingko resource accounts for 70% of the world.The effective ingredient extracted from Folium Ginkgo mainly ginkgetin etc., Semen Ginkgo pyrite its have and improve cardiovascular and cerebrovascular circulation, treatment cardiovascular and cerebrovascular disease, and improve the effects such as memory, slow down aging.Ginkgetin extraction process and ginkgoic acid content determine Semen Ginkgo product quality and price.
At present, the research of extracting ginkgetin from Folium Ginkgo is more, but there is use quantity of solvent in existing extraction process, the concentrated amount of feed liquid large mostly, be widely used in the solvent ratios of Folium Ginkgo extraction at present more than 10 times, seriously constrain the development that Folium Ginkgo extracts, shortcomings such as in this case, taking traditional production technology, when often causing extraction, inventory is few, Extraction solvent use amount is large, the concentrated amount of extracting solution is large.Extraction solvent can not fully be used, and in extracting solution, flavonoid of ginkgo biloba is saturated not, and Extraction solvent use is insufficient, causes Extraction solvent use amount large, and the concentrated amount of feed liquid is large, closely causes production cost high, and energy consumption increases.
There is the problem of ginkgoic acid too high levels in the ginkgetin that existing extraction process obtains, ginkgoic acid can not be sufficiently removed mostly, containing a large amount of ginkgoic acids in flavone product, has a strong impact on product quality.
Summary of the invention
This invention provides a kind of production technology of Folium Ginkgo extract to overcome the shortcoming of prior art, and its technique is simple, and cost is low, can greatly reduce the use amount of solvent.
The present invention solves the technical scheme that its technical problem takes: comprise the following steps: (1), extraction: by Folium Ginkgo remove impurity, whole leaf extraction; Extractant is made with the ethanol of 65-75% concentration; Solid-liquid ratio: be for the 1st time be for 1: 5, the 2nd time 1: 4, the 3rd time be 1: 3, the extract of latter twice merges the 1st time use taken turns as second, second the 2nd time of taking turns and the 3rd time use novel solvent, second rear twice extract of taking turns merges using for the 1st time as third round, so circulates; (2), concentrate: the 1st time feed liquid of each being taken turns is evaporated to soft, and thin up; (3), precipitate: add enzyme preparation, room temperature staticly settles; (4), centrifugal: by the supernatant centrifuge precipitated, to obtain centrifugal liquid; (5), resin treatment: by gained centrifugal liquid macroporous resin adsorption, with 75-80% ethanol as parsing the solvent analysis, obtain the alcoholic solution of Folium Ginkgo extract; (6), concentrated: it is 15-20% that the alcoholic solution of gained Folium Ginkgo extract is concentrated into solid content, obtains Folium Ginkgo extract desorbing concentrated solution; (7) spraying dry: will concentrate the sterilizing of gained Folium Ginkgo extract desorbing concentrated solution, carry out spraying dry, obtain the Powdered Folium Ginkgo extract of low acid, wherein ginkgetin volume content is 24%, and ginkgoic acid is less than 1ppm.
Enzyme preparation in described step (3) is that one comprises pectase, cellulase, protease and diastatic compound enzymic preparation.Described pectase, cellulase, protease and diastatic volume ratio are 2: 1: 1: 2.
The present invention is recycled by extractant, reduces the use amount of solvent, decreases the concentrated amount of extractant, reduces production cost, and whole production technology is simple, and cost is low, is applicable to suitability for industrialized production.Enzyme preparation used in the present invention is a kind of natural clarifying agent material, can significantly reduce ginkgoic acid content, play fine purification after adding clarifier.Gained powder ginkgetin unit content is 24%, and ginkgoic acid is less than 1ppm.。
Detailed description of the invention
Case study on implementation one
(1), often take turns and get 30 kg silver Folium Pruni raw materials, extract in alcoholic solution.Extract is: the ethanol of 70%; Material
Liquor ratio: be for the 1st time be for 1: 5, the 2nd time 1: 3, the 3rd time be 1: 3, the extract of latter twice merges the 1st time use taken turns as second, second the 2nd time of taking turns and the 3rd time use novel solvent, then second rear twice extract of taking turns merges using for the 1st time as third round, circulates so successively; Extraction temperature first pass extraction temperature is 75 DEG C, and second time extraction temperature is 65 DEG C, and the 3rd time extraction temperature is 65 DEG C; Extraction time is: first pass 2 hours, second time 1 hour, the 3rd time 1 hour.(2), get and respectively take turns first pass extract, utilize membrane evaporator carry out being evaporated to soft till, add water to 100L.(3), precipitate: add enzyme preparation 15g, room temperature staticly settles 2 hours.(4), centrifugal: to utilize disk plate centrifuge centrifugal the supernatant precipitated, obtain centrifugal liquid.(5), by obtained Folium Ginkgo extract centrifugal liquid carry out macroporous resin adsorption, first carry out washing and control dry, then utilizing 80% ethanol to resolve.Adsorption rate is 0.12m3/ hour, washing speed 0.22m3/ hour, resolution speed 0.12m3/ hour.(6), using membrane evaporator, desorbed solution to be concentrated into solid content be 15%, and carry out sterilizing to Folium Ginkgo extract concentrated solution, then spraying dry obtains powdery Folium Ginkgo extract product.The Folium Ginkgo extract quality of three-wheel is 0.909kg, and flavonoid of ginkgo biloba is 27.5%, ginkgoic acid 0.7ppm.
Embodiment two
(1), often take turns and get 60 kg silver Folium Pruni raw materials, extract in alcoholic solution.Extract is the ethanol of 75%; Solid-liquid ratio: be for the 1st time be for 1: 5, the 2nd time 1: 4, the 3rd time be 1: 3, the extract of latter twice merges and uses as the second the 1st time of taking turns, the second the 2nd time of taking turns and use novel solvent the 3rd time, then the second rear twice extract merging conduct taken turns
Use, circulate so successively for the 1st time of third round.Extraction temperature first pass extraction temperature is 75 DEG C, and second time extraction temperature is 65 DEG C, and the 3rd time extraction temperature is 65 DEG C; Extraction time is first pass 2 hours, second time 1 hour, the 3rd time 1 hour.(2), get and respectively take turns first pass extract, utilize membrane evaporator carry out being evaporated to soft till, add water to 200L.(3), precipitate: add enzyme preparation 30g, room temperature staticly settles 2h.(4), centrifugal: the supernatant precipitated to be utilized centrifuge, obtains centrifugal liquid.(5), by obtained Folium Ginkgo extract centrifugal liquid carry out macroporous resin adsorption, first carry out washing and control dry, then utilizing 80% ethanol to resolve.Adsorption rate is 0.09m3/ hour, washing speed 0.2m3/ hour, resolution speed 0.15m3/ hour.(6), use membrane evaporator that desorbed solution is concentrated into solid content 15%, carry out sterilizing to Folium Ginkgo extract concentrated solution, then spraying dry obtains powdery Folium Ginkgo extract product.The Folium Ginkgo extract quality of three-wheel is 1.758kg, and flavonoid of ginkgo biloba is 26.3%, ginkgoic acid 0.8ppm.
Claims (3)
1. a Folium Ginkgo extract preparation technology, is characterized in that: comprise the following steps: (1), extraction: by Folium Ginkgo remove impurity, whole leaf extraction; Extractant is made with the ethanol of 65-75% concentration; Solid-liquid ratio: be for the 1st time be for 1: 5, the 2nd time 1: 4, the 3rd time be 1: 3, the extract of latter twice merges the 1st time use taken turns as second, second the 2nd time of taking turns and the 3rd time use novel solvent, second rear twice extract of taking turns merges using for the 1st time as third round, so circulates; (2), concentrate: the 1st time feed liquid of each being taken turns is evaporated to soft, and thin up; (3), precipitate: add enzyme preparation, room temperature staticly settles; (4), centrifugal: by the supernatant centrifuge precipitated, to obtain centrifugal liquid; (5), resin treatment: by gained centrifugal liquid macroporous resin adsorption, with 75-80% ethanol as parsing the solvent analysis, obtain the alcoholic solution of Folium Ginkgo extract;
(6), concentrated: it is 15-20% that the alcoholic solution of gained Folium Ginkgo extract is concentrated into solid content, obtains Folium Ginkgo extract desorbing concentrated solution; (7) spraying dry: will concentrate the sterilizing of gained Folium Ginkgo extract desorbing concentrated solution, carry out spraying dry, obtain the Powdered Folium Ginkgo extract of low acid, wherein ginkgetin volume content is 24%, and ginkgoic acid is less than 1ppm.
2. according to the production technology of the Folium Ginkgo extract described in claim 1, it is characterized in that: the enzyme preparation in described step (3) is that one comprises pectase, cellulase, protease and diastatic compound enzymic preparation.
3. according to the production technology of the Folium Ginkgo extract described in claim 2, it is characterized in that: described pectase, cellulase, protease and diastatic volume ratio are 2: 1: 1: 2.
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CN201310440422.6A CN104435016A (en) | 2013-09-25 | 2013-09-25 | Preparation process of ginkgo leaf extract |
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CN201310440422.6A CN104435016A (en) | 2013-09-25 | 2013-09-25 | Preparation process of ginkgo leaf extract |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107048395A (en) * | 2017-03-31 | 2017-08-18 | 安徽中森生物技术有限公司 | A kind of preparation method of lowering blood pressure and blood fat composition |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107048395A (en) * | 2017-03-31 | 2017-08-18 | 安徽中森生物技术有限公司 | A kind of preparation method of lowering blood pressure and blood fat composition |
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