CN106344725A - Method for extracting flavone from herba violae - Google Patents
Method for extracting flavone from herba violae Download PDFInfo
- Publication number
- CN106344725A CN106344725A CN201610922363.XA CN201610922363A CN106344725A CN 106344725 A CN106344725 A CN 106344725A CN 201610922363 A CN201610922363 A CN 201610922363A CN 106344725 A CN106344725 A CN 106344725A
- Authority
- CN
- China
- Prior art keywords
- herba violae
- flavone
- carbon dioxide
- new method
- extraction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- 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
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/86—Violaceae (Violet family)
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0403—Solvent extraction of solutions which are liquid with a supercritical fluid
-
- 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
-
- 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
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
-
- 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
Abstract
The invention belongs to the field of natural organic chemistry and relates to a new method for extracting flavone from herba violae. The method has the following characteristics: (1) the tissue cells of herba violae are quickly and uniformly heated by a microwave technology so that the liquid in the cells is quickly vaporized to burst the cell walls so as to release the active ingredients as soon as possible; and (2) the herba violae is purified by a supercritical carbon dioxide technology so that the flavone purity exceeds 90%. Compared with the traditional technology, the method provided by the invention has the advantages of high speed, high efficiency, safety, energy saving and the like, keeps a relatively high extraction rate, greatly shortens the extraction time and reduces the impurity content in the extract. In the invention, the raw materials are widely available, the production cost is lowered, and the method is suitable for industrial production.
Description
Technical field
The invention belongs to field of natural organic chemistry, it is related to a kind of method extracting flavone from Herba Violae.
Background technology
Herba Violae (viola yedoensis makino) is Violaceae common violet platymiscium, perennial herb, also known as ground
Fourth dish, Herba Violae, arrow grass, Herba Violae, silver coin, tiger of walking alone, double-edged sword grass, Herba Violae japonicae, exempt from Auricled Hedyotis Herb, knife, little silver coin flower before gold, with dry
Dry herb enters Chinese medicine, has functions that heat-clearing and toxic substances removing, cool blood detumescence.The ground such as Herba Violae main product Jiangsu, Zhejiang, Anhui.
The chemical composition of Herba Violae mainly has flavone, coumarin, organic acid, saccharide, aminoacid, protein, Saponin, plant
Thing sterol and tannin etc., wherein, effective ingredient flavone has and improves cardiovascular and cerebrovascular circulation, spasmolytic, antiallergic and adjust new old generation
Thank, antiviral, anti-inflammation, antioxidation, antitumor etc. act on, can be used for treating coronary heart diseases and angina pectoris, presenile dementia, increasing
Strong memory, pure natural have no side effect.
At present, with Herba Violae as raw material in prior art, the method extracting flavone is decocting method, circumfluence method and ultrasonic
Method, the efficiency that macroporous adsorbent resin extracts is low, repeatability is bad, lose time, waste reagent and pollution environment etc..
Content of the invention
It is an object of the invention to provide a kind of method extracting flavone from Herba Violae, the method is using microwave extraction
Take the complex technique of technology assisted extraction flavone and supercritical carbon dioxide purification, product purity is high, low cost is easy to industrialization
Produce.
For achieving the above object, the technical solution used in the present invention is:
A kind of method extracting flavone from Herba Violae, its step is as follows:
(1) by Herba Violae cleaning, drying, 40～60 mesh sieves were pulverized；
(2) at ambient temperature, the Herba Violae of pulverizing being immersed in 60～80% ethanol (makes material and ethanol volume
Than for 1: 5～1: 15), soak 30～60min；
(3) by Herba Violae mixed liquor, in 200～400w, 30～40 DEG C, microwave extraction 15～40min；
(4) said extracted mixed liquor is put into the extractor of supercritical carbon dioxide extraction system；
(5) pressure be 25～45mpa, temperature be 35～60 DEG C under conditions of, supercritical carbon dioxide is in pressure-driven
Under, enter extractor (extraction time is 1～2h) from bottom, make flavone be dissolved in supercritical carbon dioxide, then from top together
Flow out extractor, enter knockout drum；
(6), in knockout drum, pressure is 1～2mpa, temperature is 20～25 DEG C, and the flavonoid glycoside being dissolved in carbon dioxide is isolated
Come, lodge in the bottom of knockout drum, isolate the carbon dioxide of flavonoid glycoside, then re-compress from high-pressure pump and become supercritical state
State, enters extractor；
(7) by gained flavone product, through chromatograph of liquid detection and analysis, content is more than 95%.
The inventive method has carried out following optimizations to technique scheme:
In step (1), Herba Violae is Herba Violae herb.
The inventive method has following technical effect that
(1) using microwave technology, rapid, homogeneous heating is carried out to the histiocyte of Herba Violae, make intracellular fluid fast
Speed vaporization, bursts cell wall, so that effective ingredient is discharged as soon as possible, it is excellent that the method has fast, efficient, safe, energy-conservation etc.
Point, the method, while keeping higher extraction ratio, substantially reduces the time used by extraction process, and reduces extraction
The content of impurity in liquid.
(2) utilize super critical CO 2 technology, flavone extracted, make Herba Violae flavone purity reach 90% with
On.Process is simple is easy to operate, and extraction rate is fast.
Specific embodiment
Embodiment 1
(1) by Herba Violae cleaning, drying, pulverized 40 mesh sieves, weighed 100g；
(2) at ambient temperature, the Herba Violae of pulverizing is immersed in 60% ethanol and (makes the material with ethanol volume ratio be
1: 5), soak 30min；
(3) by Herba Violae mixed liquor, in 200w, 30 DEG C, microwave extraction 5min；
(4) said extracted mixed liquor is put into the extractor of supercritical carbon dioxide extraction system；
(5) pressure is 25mpa, and temperature is 35 DEG C of supercritical carbon dioxide, enters extractor from bottom, extracts 1h；
(6) pressure be 1mpa, temperature be 20 DEG C of knockout drum in flavone is separated in uncovered plastic bottle；
(7) flavone obtained by is yellow crystalline powder, and through chromatograph of liquid detection, total flavone glucoside content is 95.15%.
Embodiment 2
(1) by Herba Violae cleaning, drying, pulverized 50 mesh sieves, weighed 100g；
(2) at ambient temperature, the Herba Violae of pulverizing is immersed in 70% ethanol and (makes the material with methanol volume ratio be
1: 10), soak 45min；
(3) by Herba Violae mixed liquor, in 300w, 35 DEG C, microwave extraction 15min；
(4) said extracted mixed liquor is put into the extractor of supercritical carbon dioxide extraction system；
(5) pressure is 32mpa, and temperature is 48 DEG C of supercritical carbon dioxide, enters extractor from bottom, extracts 1.5h；
(6) pressure be 1.5mpa, temperature be 22 DEG C of knockout drum in flavone is separated in uncovered plastic bottle；
(7) flavone obtained by is yellow crystalline powder, and through chromatograph of liquid detection, total flavone glucoside content is 95.94%.
Embodiment 3
(1) by Herba Violae cleaning, drying, pulverized 60 mesh sieves, weighed 100g；
(2) at ambient temperature, the Herba Violae of pulverizing being immersed in 80% ethanol (makes material and ethyl acetate volume
Ratio is for 1: 15), soak 60min；
(3) by Herba Violae mixed liquor, in 400w, 40 DEG C, microwave extraction 20min；
(4) said extracted mixed liquor is put into the extractor of supercritical carbon dioxide extraction system；
(5) pressure is 45mpa, and temperature is 60 DEG C of supercritical carbon dioxide, enters extractor from bottom, extracts 1.5h；
(6) pressure be 2mpa, temperature be 25 DEG C of knockout drum in flavone is separated in uncovered plastic bottle；
(7) flavone obtained by is yellow crystalline powder, and through chromatograph of liquid detection, total flavone glucoside content is 96.38%.
Claims (5)
1. a kind of new method of flavone of extracting from Herba Violae is it is characterised in that its step is as follows:
(1) by Herba Violae cleaning, drying, 40～60 mesh sieves were pulverized；
(2) at ambient temperature, the Herba Violae of pulverizing is immersed in 60～80% ethanol and (makes the material with ethanol volume ratio be
1: 5～1: 15), soak 30～60min；
(3) by Herba Violae mixed liquor, in 200～400w, 30～40 DEG C, microwave extraction 5～20min；
(4) said extracted mixed liquor is put into the extractor of supercritical carbon dioxide extraction system；
(5) pressure be 25～45mpa, temperature be 35～60 DEG C under conditions of, supercritical carbon dioxide under pressure-driven, from
Bottom enters extractor (extraction time is 1～2h), makes flavone be dissolved in supercritical carbon dioxide, then flows out extraction together from top
Take tank, enter knockout drum；
(6), in knockout drum, pressure is 1～2mpa, temperature is 20～25 DEG C, and the flavonoid glycoside being dissolved in carbon dioxide is separated, and amasss
It is stored in the bottom of knockout drum, isolates the carbon dioxide of flavonoid glycoside, then re-compress from high-pressure pump and become supercriticality, enter
Extractor；
(7) by gained flavone product, through chromatograph of liquid detection and analysis, content is more than 95%.
2. the new method extracting flavone from Herba Violae according to claim 1 is characterized in that: described step (1)
In, Herba Violae is Herba Violae herb.
3. the new method extracting flavone from Herba Violae according to claim 1 is characterized in that: described step (2)
In, 60～80% ethanol can be 60～80% methanol, ethyl acetate.
4. the new method extracting flavone from Herba Violae according to claim 1 is characterized in that: described step (6)
In, the carbon dioxide isolating flavonoid glycoside is reusable.
5. the new method extracting flavone from Herba Violae according to claim 1 is characterized in that: described step (7)
In, chromatograph of liquid is the chromatograph of liquid of subsidiary UV-detector.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610922363.XA CN106344725A (en) | 2016-10-17 | 2016-10-17 | Method for extracting flavone from herba violae |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610922363.XA CN106344725A (en) | 2016-10-17 | 2016-10-17 | Method for extracting flavone from herba violae |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106344725A true CN106344725A (en) | 2017-01-25 |
Family
ID=57863743
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610922363.XA Pending CN106344725A (en) | 2016-10-17 | 2016-10-17 | Method for extracting flavone from herba violae |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108969455A (en) * | 2018-09-04 | 2018-12-11 | 广州鹰远生物科技有限公司 | A kind of anti-acne moisture-keeping composition and its application containing viola mandshurica |
| CN109463503A (en) * | 2018-12-20 | 2019-03-15 | 株洲千金药业股份有限公司 | A kind of ampelopsis grossdentata leaf extract and its application in terms of health care product |
-
2016
- 2016-10-17 CN CN201610922363.XA patent/CN106344725A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108969455A (en) * | 2018-09-04 | 2018-12-11 | 广州鹰远生物科技有限公司 | A kind of anti-acne moisture-keeping composition and its application containing viola mandshurica |
| CN109463503A (en) * | 2018-12-20 | 2019-03-15 | 株洲千金药业股份有限公司 | A kind of ampelopsis grossdentata leaf extract and its application in terms of health care product |
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Application publication date: 20170125 |