CN108542929A - Bluish dogbane total polyphenol extract and preparation method thereof - Google Patents
Bluish dogbane total polyphenol extract and preparation method thereof Download PDFInfo
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- CN108542929A CN108542929A CN201810726909.3A CN201810726909A CN108542929A CN 108542929 A CN108542929 A CN 108542929A CN 201810726909 A CN201810726909 A CN 201810726909A CN 108542929 A CN108542929 A CN 108542929A
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- bluish dogbane
- extract
- total polyphenol
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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
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/24—Apocynaceae (Dogbane family), e.g. plumeria or periwinkle
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P9/00—Drugs for disorders of the cardiovascular system
- A61P9/12—Antihypertensives
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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
- A61K2236/55—Liquid-liquid separation; Phase separation
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Abstract
The invention discloses a kind of bluish dogbane total polyphenol extracts, it is characterised in that it is characterized in that：The content of general flavone is between 50% 85% in the extract.The present invention discloses the preparation methods of bluish dogbane total polyphenol extract, include the following steps：（1）It takes bluish dogbane medicinal powder, refluxing extraction to merge extracting solution, filters, concentration obtains concentrate；（2）Then it is colourless with water and low-concentration ethanol to be eluted to eluent respectively for macroporous resin column on concentrate；（3）Eluent is collected, ethyl alcohol is recycled, is evaporated to medicinal extract shape, it is dry, obtain bluish dogbane total polyphenol extract.
Description
Technical field
The present invention relates to pharmaceutical technology fields, and in particular to a kind of Chinese medicine bluish dogbane total polyphenol extract and its preparation side
Method.
Background technology
Bluish dogbane is the perennial herb plant of Apocynaceae Apocynum, is mainly grown in desert salt-soda soil or river
Bank, gully, hillside sandy ground, have growth in the most provinces and regions of northern China.Its leaf is simply in traditional calming liver and clearing heat
Medicine has the effect of soothing the liver tranquilizing the mind, clearing away heat and promoting diuresis, is clinically used for the diseases such as treatment neurasthenia, hypertension, ephritis edema.
Up to the present, known chemical composition mainly has flavonoids, polyphenol and organic acid etc. in document report bluish dogbane,
The study found that contained polyphenol components have apparent antihypertensive effect.Bluish dogbane preparation on the market includes that compound is spreaded out at present
Numb electuary, dogbane tea, bluish dogbane medical cigarette etc., the process of preparing of preparation is outmoded, is passed through by bluish dogbane medicinal material
Gained crude extract is prepared after simple extraction, and active constituent content is low, and it is big to take daily dosage, to reduce taking dose, improving medicine
Effect, achieve the purpose that safely, effectively, it is controllable, the present invention extracts separation using new method to bluish dogbane polyphenol, obtains higher
The extract of purity reduces taking dose to improve active constituent content in preparation, improves curative effect.
Invention content
The preparation method of bluish dogbane polyphenol extract, comprises the following steps that：
(1) the bluish dogbane medicinal material of drying and crushing is taken；
(2) ethanol solution for measuring a concentration of 40%-95% with 6-10 times is ultrasonically treated 10-60min, 40-80 DEG C of circumfluence distillation 2-
It 4 times, each 0.5-3h, centrifuges, filtering, filtrate concentration；
(3) macroporous resin column on concentrate that (2) obtain is purified, resin model D101, AB-8, LX-20, NKA-
Ⅱ、NKA-9、ADS-7；
(4) after impurity elimination being eluted with water, with 70-95% ethanol elutions；
(5) ethanol eluate is collected, is concentrated under reduced pressure, vacuum drying or freeze-drying obtain bluish dogbane total polyphenols and slightly carry after crushing
Object.
Granularity after waras crushes wherein in step (1) is 30-100 mesh.
Macroreticular resin described in step (3) is AB-8 type macroreticular resins, macroreticular resin and bluish dogbane described in step (1)
Weight ratio is 0.5-5:1.
Eluting solvent uses distilled water, 10%, 70% ethanol gradient with macroreticular resin volume ratio 5-10 to wash in step (4)
It is de-, merge 70% ethanol eluate.
The content of total polyphenols described in step (5) is between 50%-85%.
Specific implementation mode
The technical solution further illustrated the present invention below by specific implementation mode.Those skilled in the art should
It is illustrated, the embodiment is only to aid in the understanding present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
Bluish dogbane medicinal material 500g is taken, 20 mesh is crushed and sieves, 50% ethyl alcohol of 15 times of amounts of addition, refluxing extraction 2 times, 1 hour every time,
Merge extracting solution filtering, is concentrated under reduced pressure.It is processed good on concentrate（The immersion of 95% ethyl alcohol fills column, 95% alcohol flushing resin afterwards for 24 hours
Column, until efflux and distilled water 1:Until 1 mixing no longer muddiness occurs, continue with distilled water flushing resin column, until being without alcohol taste
Only）AB-8 macroporous resin columns, coutroi velocity 1mL/min, using 5mL as unit volume Fraction collection efflux, collect 50% second
Alcohol eluen is concentrated and dried, and obtains bluish dogbane total polyphenol extract, and Determination of Polyphenols is about 53%.
Embodiment 2
Bluish dogbane medicinal material 500g is taken, 40 mesh is crushed and sieves, 60% ethyl alcohol of 20 times of amounts of addition, refluxing extraction 3 times, 1 hour every time,
Merge extracting solution filtering, is concentrated under reduced pressure.It is processed good on concentrate（The immersion of 95% ethyl alcohol fills column, 95% alcohol flushing resin afterwards for 24 hours
Column, until efflux and distilled water 1:Until 1 mixing no longer muddiness occurs, continue with distilled water flushing resin column, until being without alcohol taste
Only）AB-8 macroporous resin columns, coutroi velocity 1mL/min, using 5mL as unit volume Fraction collection efflux, collect 60% second
Alcohol eluen is concentrated and dried, and obtains bluish dogbane total polyphenol extract, and Determination of Polyphenols is about 64%.
Embodiment 3
Bluish dogbane medicinal material 500g is taken, 60 mesh is crushed and sieves, 70% ethyl alcohol of 25 times of amounts of addition, refluxing extraction 4 times, 1 hour every time,
Merge extracting solution filtering, is concentrated under reduced pressure.It is processed good on concentrate（The immersion of 95% ethyl alcohol fills column, 95% alcohol flushing resin afterwards for 24 hours
Column, until efflux and distilled water 1:Until 1 mixing no longer muddiness occurs, continue with distilled water flushing resin column, until being without alcohol taste
Only）AB-8 macroporous resin columns, coutroi velocity 1mL/min, using 5mL as unit volume Fraction collection efflux, collect 70% second
Alcohol eluen is concentrated and dried, and obtains bluish dogbane total polyphenol extract, and Determination of Polyphenols is about 62%.
Embodiment 4
Bluish dogbane medicinal material 500g is taken, 40 mesh is crushed and sieves, 60% ethyl alcohol of 15 times of amounts of addition, refluxing extraction 3 times, 2 hours every time,
Merge extracting solution filtering, is concentrated under reduced pressure.It is processed good on concentrate（The immersion of 95% ethyl alcohol fills column, 95% alcohol flushing resin afterwards for 24 hours
Column, until efflux and distilled water 1:Until 1 mixing no longer muddiness occurs, continue with distilled water flushing resin column, until being without alcohol taste
Only）AB-8 macroporous resin columns, coutroi velocity 1mL/min, using 5mL as unit volume Fraction collection efflux, collect 70% second
Alcohol eluen is concentrated and dried, and obtains bluish dogbane total polyphenol extract, and Determination of Polyphenols is about 68%.
Embodiment 5
Bluish dogbane medicinal material 500g is taken, 40 mesh is crushed and sieves, 65% ethyl alcohol of 20 times of amounts of addition, refluxing extraction 3 times, 2 hours every time,
Merge extracting solution filtering, is concentrated under reduced pressure.It is processed good on concentrate（The immersion of 95% ethyl alcohol fills column, 95% alcohol flushing resin afterwards for 24 hours
Column, until efflux and distilled water 1:Until 1 mixing no longer muddiness occurs, continue with distilled water flushing resin column, until being without alcohol taste
Only）AB-8 macroporous resin columns, coutroi velocity 1mL/min, using 5mL as unit volume Fraction collection efflux, collect 70% second
Alcohol eluen is concentrated and dried, and obtains bluish dogbane total polyphenol extract, and Determination of Polyphenols is about 65%.
Claims (8)
1. a kind of bluish dogbane total polyphenol extract, it is characterised in that：The content of general flavone is between 50%-85% in the extract.
2. a kind of preparation method of bluish dogbane extractive of general flavone as described in claim 1 comprising following steps：
（1）It takes bluish dogbane medicinal powder, refluxing extraction to merge extracting solution, filters, concentration obtains concentrate；
（2）Then it is colourless with water and low-concentration ethanol to be eluted to eluent respectively for macroporous resin column on concentrate；
（3）Eluent is collected, ethyl alcohol is recycled, is evaporated to medicinal extract shape, it is dry, obtain bluish dogbane total polyphenol extract.
3. according to the method described in claim 2, it is characterized in that step（1）Described in bluish dogbane medicinal powder cross 30-100 mesh
Sieve.
4. according to the method described in claim 2, it is characterized in that step（1）Described in extracting method be with 6-10 times to measure concentration
For the ethanol solution of 40%-95%, it is ultrasonically treated 10-60min, 40-80 DEG C of circumfluence distillation 2-4 times, each 0.5-3h.
5. according to the method described in claim 2, it is characterized in that step（2）Described in macroreticular resin model D101, AB-8,
LX-20、NKA-Ⅱ、NKA-9、ADS-7。
6. according to the method described in claim 2, it is characterized in that step（2）Described in water be deionized water, water consumption is big
5-10 times of hole resin volume.
7. according to the method described in claim 2, it is characterized in that step（2）Described in low-concentration ethanol a concentration of 10%.
8. according to the method described in claim 2, it is characterized in that step（2）Described in drying means be vacuum drying or freezing
It is dry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810726909.3A CN108542929A (en) | 2018-07-05 | 2018-07-05 | Bluish dogbane total polyphenol extract and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810726909.3A CN108542929A (en) | 2018-07-05 | 2018-07-05 | Bluish dogbane total polyphenol extract and preparation method thereof |
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| CN108542929A true CN108542929A (en) | 2018-09-18 |
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| CN201810726909.3A Pending CN108542929A (en) | 2018-07-05 | 2018-07-05 | Bluish dogbane total polyphenol extract and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114224926A (en) * | 2022-01-06 | 2022-03-25 | 中国科学院新疆理化技术研究所 | Preparation method and application of effective part of apocynum venetum flower |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1634325A (en) * | 2004-11-18 | 2005-07-06 | 李青山 | Apocynum extract and extracting method thereof |
| CN101690739A (en) * | 2009-06-30 | 2010-04-07 | 长春师范学院 | Preparation method of dogbane leaf extractive |
| CN103520233A (en) * | 2013-10-24 | 2014-01-22 | 中国科学院新疆理化技术研究所 | Preparation method and application of apocynum venetum leaf total polyphenol |
| CN104546957A (en) * | 2014-12-24 | 2015-04-29 | 江苏省中国科学院植物研究所 | Water chestnut shell polyphenol extract as well as preparation method and application thereof |
-
2018
- 2018-07-05 CN CN201810726909.3A patent/CN108542929A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1634325A (en) * | 2004-11-18 | 2005-07-06 | 李青山 | Apocynum extract and extracting method thereof |
| CN101690739A (en) * | 2009-06-30 | 2010-04-07 | 长春师范学院 | Preparation method of dogbane leaf extractive |
| CN103520233A (en) * | 2013-10-24 | 2014-01-22 | 中国科学院新疆理化技术研究所 | Preparation method and application of apocynum venetum leaf total polyphenol |
| CN104546957A (en) * | 2014-12-24 | 2015-04-29 | 江苏省中国科学院植物研究所 | Water chestnut shell polyphenol extract as well as preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 石丽娟 等: "罗布麻叶总多酚纯化工艺及抗氧化活性研究", 《医药导报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114224926A (en) * | 2022-01-06 | 2022-03-25 | 中国科学院新疆理化技术研究所 | Preparation method and application of effective part of apocynum venetum flower |
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Application publication date: 20180918 |