CN104857035A - Ginkgo biloba leaf extract preparation method - Google Patents

Ginkgo biloba leaf extract preparation method Download PDF

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Publication number
CN104857035A
CN104857035A CN201510197308.4A CN201510197308A CN104857035A CN 104857035 A CN104857035 A CN 104857035A CN 201510197308 A CN201510197308 A CN 201510197308A CN 104857035 A CN104857035 A CN 104857035A
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preparation
folium ginkgo
ethanol
filtrate
obtains
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CN201510197308.4A
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欧阳玉岭
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Tianyi (tianjin) Biological Science And Technology Co Ltd
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Tianyi (tianjin) Biological Science And Technology Co Ltd
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Abstract

This invention provides a ginkgo biloba leaf extract preparation method, and belongs to the technical field of extraction and separation of natural plant effective ingredients. The preparation method is based on fresh ginkgo biloba leaf as a raw material, and includes the following steps: (1) the pretreatment of ginkgo biloba leaf into ginkgo biloba leaf powder; (2) extraction and filtering of the ginkgo biloba leaf powder to obtian a leaching solution; (3) coarse filtration and suction filtration of the leaching solution to obtain filtrate; (4) distillation and concentration of the filtrate; and (5) vacuum drying and purification of the concentrated filtrate to obtain a ginkgo biloba extract; the ginkgo biloba extract contains flavonoids and lactone. The preparation method simplifies the production process, and is less in steps, simple in operation, free of use of a lot of organic solvent, high in recovery rate, and non-pollution.

Description

A kind of preparation method of Folium Ginkgo extract
Technical field
The invention relates to natural plants active ingredient extraction and separation technology field, is specifically related to a kind of preparation method of Folium Ginkgo extract.
Background technology
Semen Ginkgo is Ginkgoaceae, Ginkgo deciduous tree.Before Semen Ginkgo appears at several hundred million years, be Relict Plant the most ancient in the gymnosperm that carries over after quaternary glacier motion, the alive Semen Ginkgo of existing work is rare and disperse, and upper veteran at the age of one hundred years old is rare, all become extinct, so Semen Ginkgo has again the laudatory title of living fossil with its every other plant with guiding principle.The materials such as the rare a large amount of ginkgetin of Folium Ginkgo extract and bilobalide, it can increase cerebrovascular flow, improves Cerebrovascular disorders function; protection brain cell, coronary artery dilator, prevents angina pectoris and myocardial infarction; prevent thrombosis, improve body immunity.Very useful per capita to coronary heart diseases and angina pectoris, cerebral arteriosclerosis, alzheimer disease, hypertension.
Extracting method of the prior art comprises:
1, organic solvent extraction: current the most widely used Folium Ginkgo extracting method, conventional volume system comprises alcohol-water or acetone-water carries out lixiviate, but does not confirm in existing document which kind of organic solvent is best volume, still needs further investigation.
2, steam distillation: it is simple that the method has equipment, and cost is low, and meets environmental requirement, but in prior art, water extraction extraction efficiency is low, and impurity content is high, aftertreatment technology difficulty is large, therefore applies less.
3, additive method: comprise super-critical fluid extraction, microwave loss mechanisms, ultrasonic extraction, high-speed countercurrent chromatography extraction method, the extracting method such as cell and tissue culture synthetic method and enzyme process.It is high that these technology have the response rate, the free of contamination feature of environmental protection, but due to the reason such as cost, technology, also under test, not mature enough.
Traditional extracting method, solvent easily or faster enters cell under the condition of heating, but solable matter is higher at the condition dissolubility of heat, successively occurred very high osmotic pressure by dissolving, cause extraction ratio low, active component is low, and technique is loaded down with trivial details, the production cycle is long.
Novel extracting method, also under test, cost is high, operates more difficult, describedly still can not be applicable to industrialized large-scale production at present.
Summary of the invention
The problem that the invention will solve is for the problems referred to above, is optimized by traditional more ripe extracting method, the preparation method of that design a kind of simplification, that extraction ratio is high Folium Ginkgo extract.
For solving the problems of the technologies described above, the technical scheme that the invention adopts is: a kind of preparation method of Folium Ginkgo extract, and with fresh Folium Ginkgo for raw material, its preparation method comprises:
(1) pretreatment of Folium Ginkgo: fresh Folium Ginkgo is cleaned, dries, is crushed to powder;
(2) lixiviate: the Ginkgo Leaf alcohol steep that step (1) is obtained, the proportioning of Ginkgo Leaf and ethanol presses the weight of Ginkgo Leaf: the volume=1:7 of ethanol, filter, filtering residue is used alcohol steep again, the proportioning of filtering residue and ethanol presses the weight of filtering residue: volume=1:7 ~ 8 of ethanol, filter, merge lixiviating solution;
(3) sucking filtration: carried out by the lixiviating solution that step (2) obtains filtering, sucking filtration, obtains filtrate;
(4) distill, concentrate: the filtrate that step (3) obtains is concentrated, obtains concentrated filtrate;
(5) dry: the concentrated filtrate that step (4) obtains to be carried out drying, purification, obtains extract.
Further, Folium Ginkgo described in step (1) dries 8 ~ 12h in 70 DEG C, and described ginkgo leaf powder is broken to 60 orders.
Further, described in step (2), ethanol contend concentration is 60%, with 640ml 95% ethanol and 360ml pure water formulated.
Further, Ginkgo Leaf described in step (2) soaks in ethanol in 60 DEG C ~ 70 DEG C insulations 2 hours, timing agitation, and described filtering residue soaks in ethanol in 60 DEG C ~ 70 DEG C insulations 2 hours, timing agitation.
Further, repeat step (2) and do parallel laboratory test.
Further, in step (3), first lixiviating solution gauze coarse filtration is obtained coarse filtration liquid, then coarse filtration liquid is joined in the buchner funnel with filter paper and carry out sucking filtration, obtain filtrate.
Further, concentrated filtrate described in step (5) carries out 60 DEG C ~ 70 DEG C vacuum dryings.
Further, described in step (5), extract comprises flavonoid and lactone.
The advantage that the invention has and good effect are:
1, the preparation method of Folium Ginkgo extract in the invention, adopts ethanol as extractant, adopts twice lixiviates in 2 hours, compared with prior art simplify experimental procedure, not only save a large amount of organic or inorganic solvents, and effectively reduce costs and environmental pollution, operation has safety.
2, the alcoholic solution that in the invention, leaching process is only 60% simply by employing volumetric concentration carries out lixiviate, and under guarantee has the prerequisite of higher extracted rate, compared with other organic solvents, the response rate is high, pollution-free.
3, first adopt gauze coarse filtration to go out bulky grain deposit in the invention in sucking filtration step, reduce the blocking that gelatinous precipitate in Folium Ginkgo is easy to filter paper, contribute to the speed improving next step sucking filtration.
4, the invention has and simplifies production technology, and step is few, easy and simple to handle, does not need to use a large amount of organic solvents, and the response rate is high, not have the feature of pollution.
Detailed description of the invention
Below the specific embodiment of the invention is illustrated:
Calculate the method for yield: take dry empty surface plate m (g), extract is placed on culture dish and weighs m 1g (), the Ginkgo Leaf of 100g drying, then extract GBE content is: extract yield=(m 1-m)/100 × 100%.
Embodiment 1
A preparation method for Folium Ginkgo extract, with fresh Folium Ginkgo for raw material, its preparation method comprises:
The pretreatment of Folium Ginkgo: get fresh Folium Ginkgo and clean and dry, dry 8 hours in 70 DEG C of baking ovens, take out and be placed in cooling in drying baker, the ginkgo leaf powder of drying is broken to 60 orders, and it is stand-by that Ginkgo Leaf is placed in brown, wide-mouth bottle;
Lixiviate: volumetric concentration be 60% alcoholic solution with 640ml 95% ethanol and 360ml pure water formulated.Get 100g Ginkgo Leaf and be placed in the alcoholic solution that 700ml volumetric concentration is 60%, be placed in the water-bath lixiviate 2h of 60 DEG C, stirred once every 10 minutes, by filtered through gauze, filtering residue adds 700ml alcoholic solution again, be placed in the water-bath lixiviate 2h of 60 DEG C, stirred once every 10 minutes, lixiviate terminates, filtered through gauze, merge lixiviating solution, do parallel laboratory test simultaneously;
Sucking filtration: first lixiviating solution gauze coarse filtration is obtained coarse filtration liquid, then install Suction filtration device, joined by coarse filtration liquid in the buchner funnel with filter paper and carry out sucking filtration, a sucking filtration process changes the filter paper of buchner funnel described in multiple, obtains filtrate and abandons filtering residue;
Distill, concentrate: filtrate carries out concentrated employing distillation, enrichment facility, concentrates, obtain concentrated filtrate to filtrate;
Dry: concentrated filtrate to be carried out vacuum drying with 60 DEG C, purification, large vacuum reduces boiling point, and remove last ethanol and residual portion of water, obtain extract, described extract comprises flavonoid and lactone.The yield 25.36% of described extract.
Embodiment 2
A preparation method for Folium Ginkgo extract, with fresh Folium Ginkgo for raw material, its preparation method comprises:
The pretreatment of Folium Ginkgo: get fresh Folium Ginkgo and clean and dry, dry 10 hours in 70 DEG C of baking ovens, take out and be placed in cooling in drying baker, the ginkgo leaf powder of drying is broken to 60 orders, and it is stand-by that Ginkgo Leaf is placed in brown, wide-mouth bottle;
Lixiviate: volumetric concentration be 60% alcoholic solution with 640ml 95% ethanol and 360ml pure water formulated.Get 200g Ginkgo Leaf and be placed in the alcoholic solution that 1400ml volumetric concentration is 60%, be placed in the water-bath lixiviate 2h of 65 DEG C, stirred once every 10 minutes, by filtered through gauze, filtering residue adds 1400ml alcoholic solution again, be placed in the water-bath lixiviate 2h of 65 DEG C, stirred once every 10 minutes, lixiviate terminates, filtered through gauze, merge lixiviating solution, do parallel laboratory test simultaneously;
Sucking filtration: first lixiviating solution gauze coarse filtration is obtained coarse filtration liquid, then install Suction filtration device, joined by coarse filtration liquid in the buchner funnel with filter paper and carry out sucking filtration, a sucking filtration process changes the filter paper of buchner funnel described in multiple, obtains filtrate and abandons filtering residue;
Distill, concentrate: filtrate carries out concentrated employing distillation, enrichment facility, concentrates, obtain concentrated filtrate to filtrate;
Dry: concentrated filtrate to be carried out vacuum drying with 65 DEG C, purification, large vacuum reduces boiling point, and remove last ethanol and residual portion of water, obtain extract, described extract comprises flavonoid and lactone.The yield 28.12% of described extract
Embodiment 3
A preparation method for Folium Ginkgo extract, with fresh Folium Ginkgo for raw material, its preparation method comprises:
The pretreatment of Folium Ginkgo: get fresh Folium Ginkgo and clean and dry, dry 12 hours in 70 DEG C of baking ovens, take out and be placed in cooling in drying baker, the ginkgo leaf powder of drying is broken to 60 orders, and it is stand-by that Ginkgo Leaf is placed in brown, wide-mouth bottle;
Lixiviate: volumetric concentration be 60% alcoholic solution with 640ml 95% ethanol and 360ml pure water formulated.Get 300g Ginkgo Leaf and be placed in the alcoholic solution that 2100ml volumetric concentration is 60%, be placed in the water-bath lixiviate 2h of 70 DEG C, stirred once every 10 minutes, by filtered through gauze, filtering residue adds 2100ml alcoholic solution again, be placed in the water-bath lixiviate 2h of 70 DEG C, stirred once every 10 minutes, lixiviate terminates, filtered through gauze, merge lixiviating solution, do parallel laboratory test simultaneously;
Sucking filtration: first lixiviating solution gauze coarse filtration is obtained coarse filtration liquid, then install Suction filtration device, joined by coarse filtration liquid in the buchner funnel with filter paper and carry out sucking filtration, a sucking filtration process changes the filter paper of buchner funnel described in multiple, obtains filtrate and abandons filtering residue;
Distill, concentrate: filtrate carries out concentrated employing distillation, enrichment facility, concentrates, obtain concentrated filtrate to filtrate;
Dry: concentrated filtrate to be carried out vacuum drying with 70 DEG C, purification, large vacuum reduces boiling point, and remove last ethanol and residual portion of water, obtain extract, described extract comprises flavonoid and lactone.The yield 30.22% of described extract.
Above the embodiment of the invention has been described in detail, but described content being only the preferred embodiment of the invention, the practical range for limiting the invention can not being considered to.All equalizations done according to the invention scope change and improve, and all should still belong within this patent covering scope.

Claims (8)

1. a preparation method for Folium Ginkgo extract, is characterized in that: with fresh Folium Ginkgo for raw material, its preparation method comprises:
(1) pretreatment of Folium Ginkgo: fresh Folium Ginkgo is cleaned, dries, is crushed to powder;
(2) lixiviate: the Ginkgo Leaf alcohol steep that step (1) is obtained, the proportioning of Ginkgo Leaf and ethanol presses the weight of Ginkgo Leaf: the volume=1:7 of ethanol, filter, filtering residue is used alcohol steep again, the proportioning of filtering residue and ethanol presses the weight of filtering residue: volume=1:7 ~ 8 of ethanol, filter, merge lixiviating solution;
(3) sucking filtration: carried out by the lixiviating solution that step (2) obtains filtering, sucking filtration, obtains filtrate;
(4) distill, concentrate: the filtrate that step (3) obtains is concentrated, obtains concentrated filtrate;
(5) dry: the concentrated filtrate that step (4) obtains to be carried out drying, purification, obtains extract.
2. the preparation method of a kind of Folium Ginkgo extract according to claim 1, is characterized in that: Folium Ginkgo described in step (1) dries 8 ~ 12h in 70 DEG C, and described ginkgo leaf powder is broken to 60 orders.
3. the preparation method of a kind of Folium Ginkgo extract according to claim 1, is characterized in that: described in step (2), ethanol contend concentration is 60%, with 640ml 95% ethanol and 360ml pure water formulated.
4. the preparation method of a kind of Folium Ginkgo extract according to claim 1, it is characterized in that: Ginkgo Leaf described in step (2) soaks in ethanol in 60 DEG C ~ 70 DEG C insulations 2 hours, timing agitation, described filtering residue soaks in ethanol in 60 DEG C ~ 70 DEG C insulations 2 hours, timing agitation.
5. the preparation method of a kind of Folium Ginkgo extract according to claim 1, is characterized in that: repeat step (2) and do parallel laboratory test.
6. the preparation method of a kind of Folium Ginkgo extract according to claim 1, it is characterized in that: in step (3), first lixiviating solution gauze coarse filtration is obtained coarse filtration liquid, again coarse filtration liquid is joined in the buchner funnel with filter paper and carry out sucking filtration, obtain filtrate.
7. the preparation method of a kind of Folium Ginkgo extract according to claim 1, is characterized in that: concentrated filtrate described in step (5) carries out 60 DEG C ~ 70 DEG C vacuum dryings.
8. the preparation method of a kind of Folium Ginkgo extract according to claim 1, is characterized in that: described in step (5), extract comprises flavonoid and lactone.
CN201510197308.4A 2015-04-24 2015-04-24 Ginkgo biloba leaf extract preparation method Pending CN104857035A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105833571A (en) * 2016-03-22 2016-08-10 湖州国信物资有限公司 Preparation method and application of novel defoaming agent
CN106581089A (en) * 2016-12-28 2017-04-26 成都景睿生物科技有限公司 Preparation method of folium ginkgo extract
CN110420552A (en) * 2019-08-09 2019-11-08 北京泷涛环境修复有限公司 A kind of plant deodorant and preparation method for the processing of solid waste waste odor
RU2778292C1 (en) * 2018-08-20 2022-08-17 Спх Син Лин Сай. & Тек. Фармасьютикал Ко., Лтд. Granular complex ketone ether of ginkgo biloba and method for its preparation
CN116808085A (en) * 2023-07-31 2023-09-29 宁波大学科学技术学院 Method for extracting ginkgo leaf flavone by membrane separation and flavone determination method

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1448172A (en) * 2003-04-30 2003-10-15 江苏扬子江药业集团有限公司 Folium ginkgo injection and preparation thereof
CN101049324A (en) * 2006-04-07 2007-10-10 黄振华 Composition of medication prepared from ginkgo leaves and puerarin
CN103751230A (en) * 2013-09-11 2014-04-30 王青 Application of gingko extract nanometer liposome in gynecological disease treatment

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1448172A (en) * 2003-04-30 2003-10-15 江苏扬子江药业集团有限公司 Folium ginkgo injection and preparation thereof
CN101049324A (en) * 2006-04-07 2007-10-10 黄振华 Composition of medication prepared from ginkgo leaves and puerarin
CN103751230A (en) * 2013-09-11 2014-04-30 王青 Application of gingko extract nanometer liposome in gynecological disease treatment

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105833571A (en) * 2016-03-22 2016-08-10 湖州国信物资有限公司 Preparation method and application of novel defoaming agent
CN106581089A (en) * 2016-12-28 2017-04-26 成都景睿生物科技有限公司 Preparation method of folium ginkgo extract
RU2778292C1 (en) * 2018-08-20 2022-08-17 Спх Син Лин Сай. & Тек. Фармасьютикал Ко., Лтд. Granular complex ketone ether of ginkgo biloba and method for its preparation
CN110420552A (en) * 2019-08-09 2019-11-08 北京泷涛环境修复有限公司 A kind of plant deodorant and preparation method for the processing of solid waste waste odor
CN116808085A (en) * 2023-07-31 2023-09-29 宁波大学科学技术学院 Method for extracting ginkgo leaf flavone by membrane separation and flavone determination method

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