CN106109510A - Fine silver flavone extraction process - Google Patents
Fine silver flavone extraction process Download PDFInfo
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- CN106109510A CN106109510A CN201610054491.7A CN201610054491A CN106109510A CN 106109510 A CN106109510 A CN 106109510A CN 201610054491 A CN201610054491 A CN 201610054491A CN 106109510 A CN106109510 A CN 106109510A
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- ethyl acetate
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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
- 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
- A61K2236/35—Extraction with lipophilic solvents, e.g. Hexane or petrol ether
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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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Abstract
The embodiment of the invention discloses a kind of fine silver flavone extraction process, it comprises the steps that raw material Folium Ginkgo extract is dissolved in water by (1)；It is centrifuged Folium Ginkgo extract solution separating, collects filtrate；Filtering residue is dissolved, is centrifuged and collects filtrate；(2) filtrate in step (1) is extracted, phase raffinate of fetching water；(3) being extracted by aqueous phase raffinate in step (2), take ester phase extract, by extract concentrating under reduced pressure, the extract after concentrating carries out lyophilization, obtains Refined flavonoid powder；Technical scheme disclosed in this invention can be effective and rapid and stable by the extracting flavonoids in Folium Ginkgo extract out, the total flavones average content of final extract is far above similar-type products on market, and the extractant low cost used, recyclable, reduce production cost, it is adaptable to promote the use of.
Description
Technical field
The present invention relates to a kind of fine silver flavone extraction process.
Background technology
Semen Ginkgo, has another name called maidenhair tree, Gong Sunshu, is China's endemic tree.The leaf of Semen Ginkgo, really, bark all can be used as medicine, the medical value of You Yiye is the highest.The chemical composition of Folium Ginkgo is complex; its extract mainly contains flavone compound and diterpene-kind compound; ginkgetin can increase cerebrovascular blood flow; improve blood brain vascular circulation function; protection brain cell, coronary artery dilator, prevention angina pectoris and myocardial infarction; antithrombotic, improves body immunity.
The extracting method of existing Folium Ginkgo flavone compounds has organic solvent extraction, super critical point purification method, water extraction method, but it is low all to there is extraction ratio, the defect that cost is high.
Due to the medical value that ginkgetin is high so that it is extracting method becomes one of the much-talked-about topic in research and development field both at home and abroad, how can improve its extraction ratio, reduces extraction cost, becomes the problem that numerous scientific research institution pays close attention to always.
Summary of the invention
The present invention is directed to prior art not enough, it is provided that fine silver flavone extraction process, its extraction efficiency is high, and effectively reduces extraction cost, thus effectively reduces production cost.
Adopt the following technical scheme that to reach the above-mentioned technique effect present invention
A kind of fine silver flavone extraction process, comprises the steps:
(1) raw material Folium Ginkgo extract is added in the water of 30 DEG C ~ 75 DEG C, dissolve, form Folium Ginkgo extract solution；
It is centrifuged Folium Ginkgo extract solution separating, collects filtrate；The disodium phosphate soln that filtering residue concentration is 0.1% ~ 0.15% is dissolved at 55 DEG C ~ 60 DEG C, is centrifuged and collects filtrate；
Merge above-mentioned filtrate；
(2) the filtrate pH after merging in step (1) is adjusted to 4.5 ~ 5.0, then adds isopyknic organic solvent I in this filtrate and extract, phase raffinate of fetching water；
Described organic solvent I is ethyl acetate and petroleum ether mixed solution or ethyl acetate and normal heptane mixed solution, and the volume ratio of described ethyl acetate and the volume ratio of petroleum ether or ethyl acetate and normal heptane is 3:1 ~ 6:1；
(3) aqueous phase raffinate pH in step (2) is adjusted to 6.50 ~ 8.50, in aqueous phase raffinate, add isopyknic organic solvent II extract, take ester phase extract, by extract concentrating under reduced pressure, extract after concentrating carries out lyophilization, obtains Refined flavonoid powder；
Described organic solvent II includes that ethyl acetate and n-butyl alcohol, the volume ratio of described ethyl acetate and n-butyl alcohol are 3:1 ~ 6:1.
As preferably, described step (1) water temperature is 55 DEG C, and described raw material Folium Ginkgo extract is 1g/20ml-25ml with the mass body volume concentrations (w/v) of water.
As preferably, in described step (2), the volume ratio of ethyl acetate and the volume ratio of petroleum ether or ethyl acetate and normal heptane is 4:1.
As preferably, described step 2 uses phosphoric acid,diluted and sodium hydroxide combination or dilute hydrochloric acid and sodium hydroxide combination.
As preferably, in described step (3), raffinate pH value is 7.5.
As preferably, in described organic solvent II, ethyl acetate is 4:1 with the volume ratio of n-butyl alcohol.
As preferably, described dissolving water is water for injection.
The present invention provides a kind of fine silver flavone extraction process, comprises the steps:
(1) being added by raw material Folium Ginkgo extract in the water of 30 DEG C ~ 75 DEG C, ultrasonic wave concussion dissolves, and forms Folium Ginkgo extract solution；
It is centrifuged Folium Ginkgo extract solution separating, collects filtrate；By disodium phosphate soln ultrasonic dissolution at 55 DEG C ~ 60 DEG C that filtering residue concentration is 0.1% ~ 0.15%, it is centrifuged and collects filtrate；
Merge above-mentioned filtrate；
(2) the filtrate pH after merging in step (1) is adjusted to 4.5 ~ 5.0, then adds isopyknic organic solvent I in this filtrate and extract, phase raffinate of fetching water；
Described organic solvent I is ethyl acetate and petroleum ether mixed solution or ethyl acetate and normal heptane mixed solution, and the volume ratio of described ethyl acetate and the volume ratio of petroleum ether or ethyl acetate and normal heptane is 3:1 ~ 6:1；
(3) aqueous phase raffinate pH in step (2) is adjusted to 6.50 ~ 8.50, in aqueous phase raffinate, add isopyknic organic solvent II extract, take ester phase extract, by extract concentrating under reduced pressure, extract after concentrating carries out lyophilization, obtains Refined flavonoid powder；
Described organic solvent II includes that ethyl acetate and n-butyl alcohol, the volume ratio of described ethyl acetate and n-butyl alcohol are 3:1 ~ 6:1.
Technical scheme disclosed in this invention can be effective and rapid and stable by the extracting flavonoids in Folium Ginkgo extract out, the total flavones average content of final extract is far above similar-type products on market, and the extractant low cost used, recyclable, reduce production cost, it is adaptable to promote the use of.
The embodiment of the invention discloses a kind of fine silver flavone extraction process.Those skilled in the art can use for reference present disclosure, is suitably modified technological parameter and realizes.Special needs to be pointed out is, all similar replacements and change apparent to those skilled in the art, they are considered as being included in the present invention.The product of the present invention is described by preferred embodiment, and related personnel substantially can be to product as herein described in without departing from present invention, spirit and scope
It is modified with method or suitably changes and combine, realize and apply the technology of the present invention.
In order to be further appreciated by the present invention, below in conjunction with embodiment, the present invention is described in detail.
Detailed description of the invention
Embodiment 1
A kind of fine silver flavone extraction process, it comprises the steps:
(1) will add the water of 55 DEG C in raw material Folium Ginkgo extract, ultrasonic wave concussion dissolves 2min, forms Folium Ginkgo extract solution；Described raw material Folium Ginkgo extract is 1g, and water is 20mL, and described raw material Folium Ginkgo extract is 1g/20ml with the mass body volume concentrations (w/v) of water；
It is centrifuged Folium Ginkgo extract solution separating, collects filtrate；Filtering residue 0.1% disodium phosphate soln ultrasonic dissolution at 55 DEG C is dissolved 15min, is centrifuged and collects filtrate；
Merge the filtrate obtained for twice；
(2) pH is adjusted to 4.5 ~ 5.0 by filtrate phosphoric acid,diluted after merging in step (1) and sodium hydroxide solution, then adds isopyknic organic solvent I in this filtrate and carry out extracting 3 times, phase raffinate of fetching water；Wherein ester is separated and collects standby, uses in other operation；
Described organic solvent I includes that ethyl acetate and petroleum ether, described ethyl acetate are 4:1 with the volume ratio of petroleum ether；(agent combination adjusting pH can be replaced by dilute hydrochloric acid and sodium hydroxide combination)；
(3) diluted sodium hydroxide solution of aqueous phase raffinate in step (2) is adjusted pH to 7.5, in aqueous phase raffinate, add isopyknic organic solvent II carry out extracting 3 times, merge ester phase extract, extract concentrating under reduced pressure after merging recycling design, extract after concentrating carries out lyophilization, obtains Refined flavonoid powder；The above organic solvent II includes that ethyl acetate and n-butyl alcohol, the volume ratio of described ethyl acetate and n-butyl alcohol are 4:1.
Embodiment 2
A kind of fine silver flavone extraction process, it comprises the steps:
(1) will add the water of 30 DEG C in raw material Folium Ginkgo extract, ultrasonic vibration dissolves 2min, forms Folium Ginkgo extract solution；Described raw material Folium Ginkgo extract is 1g, and water is 20mL, and described raw material Folium Ginkgo extract is 50g/L with the mass body volume concentrations (w/v) of water；
It is centrifuged Folium Ginkgo extract solution separating, collects filtrate；By filtering residue 0.1% disodium phosphate soln ultrasonic dissolution 15min at 55 DEG C, it is centrifuged and collects filtrate；
Merge above-mentioned filtrate；
(2) the filtrate pH after merging in step (1) is adjusted to 4.5 ~ 5.0, then adds isopyknic organic solvent I in this filtrate and carry out extracting 3 times, phase raffinate of fetching water；
Described organic solvent I includes that ethyl acetate and petroleum ether, described ethyl acetate are 3:1 with the volume ratio of petroleum ether；
(3) diluted sodium hydroxide solution of aqueous phase raffinate in step (2) is adjusted pH to 6.50, in aqueous phase raffinate, add isopyknic organic solvent II carry out extracting 3 times, merge ester phase extract, extract concentrating under reduced pressure after merging recycling design, extract after concentrating carries out lyophilization, obtains Refined flavonoid powder；
The above organic solvent II includes that ethyl acetate and n-butyl alcohol, the volume ratio of described ethyl acetate and n-butyl alcohol are 3:1.
Embodiment 3
A kind of fine silver flavone extraction process, it comprises the steps:
(1) will add the water of 75 DEG C in raw material Folium Ginkgo extract, ultrasonic wave concussion dissolves 2min, forms Folium Ginkgo extract solution；Described raw material Folium Ginkgo extract is 1g, and water is 20mL, and described raw material Folium Ginkgo extract is 50g/L with the mass body volume concentrations (w/v) of water；
It is centrifuged Folium Ginkgo extract solution separating, collects filtrate；By filtering residue 0.1% disodium phosphate soln ultrasonic dissolution 15min at 60 DEG C, it is centrifuged and collects filtrate；
Merge above-mentioned filtrate；
(2) the filtrate pH after merging in step (1) is adjusted to 4.5 ~ 5.0, then adds isopyknic organic solvent I in this filtrate and carry out extracting 3 times, phase raffinate of fetching water；
Described organic solvent I includes that ethyl acetate and petroleum ether, described ethyl acetate are 6:1 with the volume ratio of petroleum ether；
(3) diluted sodium hydroxide solution of aqueous phase raffinate in step (2) is adjusted pH to 8.50, in aqueous phase raffinate, add isopyknic organic solvent II carry out extracting 3 times, merge ester phase extract, extract concentrating under reduced pressure after merging, extract after concentrating carries out lyophilization, obtains Refined flavonoid powder；
The above organic solvent II includes that ethyl acetate and n-butyl alcohol, the volume ratio of described ethyl acetate and n-butyl alcohol are 6:1.
Embodiment 4
The present embodiment is reference examples, is wherein relative to embodiment 1 ~ 3 difference: described raw material Folium Ginkgo extract is 1g, and water is 25mL, and described raw material Folium Ginkgo extract is 40g/L with the mass body volume concentrations (w/v) of water.
Embodiment 5
The present embodiment is reference examples, is wherein relative to embodiment 1 ~ 3 difference: machine solvent I is ethyl acetate and normal heptane.
In above example, used dissolving water is water for injection, the ratio of the described i.e. Solute mass of mass body volume concentrations and solvent volume, i.e. w/v.
" Folium Ginkgo extract " used in above example is the raw material meeting national standard, its active constituent content: ginkgetin is (with reference to relevant national standard methods analyst, calculate with Quercetin, kaempferol and isorhamnetin for reference substance), content is not less than 24%；Bilobalide (calculates with Ginkgolide A. B. C and bilobalide total amount), and content is not less than 6%.The content of ginkgoic acid is less than national standard.
Being 46.14% by measuring the total flavones average content of the final products that embodiment 1 obtains, the total flavones average content in the final products that embodiment 2 obtains is 42.60%, and in the end product that embodiment 3 obtains, total flavones average content is 41.56%；The content of above example total flavones is above the general flavone content 28% ~ 33.5% of similar-type products on market.Embodiment 4 is identical with average general flavone content in the product obtained by the embodiment compareed accordingly with product obtained by embodiment 5, and i.e. both final total flavones average content differences that measure are 0.01% ~ 0.05%, meet experiment allowable error value.
Comparative example 1 ~ 3, it is clear that the product total flavones average content obtained by embodiment 1 is significantly larger than the general flavone content of similar-type products on market, and its total flavones average content is far above the total flavones average content of other embodiments.
Table 1 measures for embodiment 1 products obtained therefrom HPLC, obtains Folium Ginkgo and refines the assay result of total flavones in extract.
Total flavones average content result in table 1 embodiment 1 product
The above is only the preferred embodiment of the present invention; it should be pointed out that, for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (7)
1. a fine silver flavone extraction process, it is characterised in that it comprises the steps:
(1) raw material Folium Ginkgo extract is added in the water of 30 DEG C ~ 75 DEG C, dissolve, form Folium Ginkgo extract solution；
It is centrifuged Folium Ginkgo extract solution separating, collects filtrate；The disodium phosphate soln that filtering residue concentration is 0.1% ~ 0.15% is dissolved at 55 DEG C ~ 60 DEG C, is centrifuged and collects filtrate；
Merge above-mentioned filtrate；
(2) the filtrate pH after merging in step (1) is adjusted to 4.5 ~ 5.0, then adds isopyknic organic solvent I in this filtrate and extract, phase raffinate of fetching water；
Described organic solvent I is ethyl acetate and petroleum ether mixed solution or ethyl acetate and normal heptane mixed solution, and the volume ratio of described ethyl acetate and the volume ratio of petroleum ether or ethyl acetate and normal heptane is 3:1 ~ 6:1；
Adjusting aqueous phase raffinate pH in step (2) to 6.50 ~ 8.50, add isopyknic organic solvent II and extract, take ester phase extract in aqueous phase raffinate, by extract concentrating under reduced pressure, the extract after concentrating carries out lyophilization, obtains Refined flavonoid powder；
Described organic solvent II includes that ethyl acetate and n-butyl alcohol, the volume ratio of described ethyl acetate and n-butyl alcohol are 3:1 ~ 6:1.
Fine silver flavone extraction process the most according to claim 1, it is characterised in that described step (1) water temperature is 55 DEG C, described raw material Folium Ginkgo extract is 50g/L ~ 40g/L with the mass body volume concentrations of water.
Fine silver flavone extraction process the most according to claim 1, it is characterised in that in described step (2), the volume ratio of ethyl acetate and the volume ratio of petroleum ether or ethyl acetate and normal heptane is 4:1.
4. according to the fine silver flavone extraction process described in claim 1,2 or 3, it is characterised in that described step 2 uses phosphoric acid,diluted and sodium hydroxide combination or dilute hydrochloric acid and sodium hydroxide combination.
5. according to the fine silver flavone extraction process described in claim 1,2 or 3 any one, it is characterised in that in described step (3), raffinate pH value is 7.5.
6. according to the fine silver flavone extraction process described in claim 1 ~ 3 any one, it is characterised in that in described organic solvent II, ethyl acetate is 4:1 with the volume ratio of n-butyl alcohol.
Fine silver flavone extraction process the most according to claim 5, it is characterised in that in described organic solvent II, ethyl acetate is 4:1 with the volume ratio of n-butyl alcohol.
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| CN201610054491.7A CN106109510A (en) | 2016-01-27 | 2016-01-27 | Fine silver flavone extraction process |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106727491A (en) * | 2016-12-08 | 2017-05-31 | 河北润茂制药有限公司 | A kind of Bilobanoate medicinal raw material |
| WO2019113861A1 (en) * | 2017-12-13 | 2019-06-20 | 巴卫松 | Ginkgo biloba extract medicinal raw material and preparation method therefor |
| CN110361346A (en) * | 2019-07-19 | 2019-10-22 | 浙江大学 | A kind of quality determining method of dendrobium candidum medicinal material |
| CN115594654A (en) * | 2022-10-28 | 2023-01-13 | 河北荃美生物科技有限公司（Cn） | Extraction method and application of 7-demethyl ginkgetin and ginkgetin ester |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101199560A (en) * | 2007-12-27 | 2008-06-18 | 扬子江药业集团有限公司 | Ginkgo leaf extract and preparing method thereof |
| CN101780122A (en) * | 2010-02-23 | 2010-07-21 | 广州汉方现代中药研究开发有限公司 | Preparation method of a water-soluble gingko extract |
| CN101904877A (en) * | 2010-08-06 | 2010-12-08 | 合肥工业大学 | New preparation method of low-phenolic acid gingko flavone extractive |
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2016
- 2016-01-27 CN CN201610054491.7A patent/CN106109510A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101199560A (en) * | 2007-12-27 | 2008-06-18 | 扬子江药业集团有限公司 | Ginkgo leaf extract and preparing method thereof |
| CN101780122A (en) * | 2010-02-23 | 2010-07-21 | 广州汉方现代中药研究开发有限公司 | Preparation method of a water-soluble gingko extract |
| CN101904877A (en) * | 2010-08-06 | 2010-12-08 | 合肥工业大学 | New preparation method of low-phenolic acid gingko flavone extractive |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106727491A (en) * | 2016-12-08 | 2017-05-31 | 河北润茂制药有限公司 | A kind of Bilobanoate medicinal raw material |
| WO2019113861A1 (en) * | 2017-12-13 | 2019-06-20 | 巴卫松 | Ginkgo biloba extract medicinal raw material and preparation method therefor |
| CN110198713A (en) * | 2017-12-13 | 2019-09-03 | 巴卫松 | A kind of ginkgo biloba extract medicinal raw material and preparation method thereof |
| CN110361346A (en) * | 2019-07-19 | 2019-10-22 | 浙江大学 | A kind of quality determining method of dendrobium candidum medicinal material |
| CN115594654A (en) * | 2022-10-28 | 2023-01-13 | 河北荃美生物科技有限公司（Cn） | Extraction method and application of 7-demethyl ginkgetin and ginkgetin ester |
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