CN102603826A - Method for extracting 8-acetylharpagide from decumbent bugle herb plant - Google Patents
Method for extracting 8-acetylharpagide from decumbent bugle herb plant Download PDFInfo
- Publication number
- CN102603826A CN102603826A CN2011100227030A CN201110022703A CN102603826A CN 102603826 A CN102603826 A CN 102603826A CN 2011100227030 A CN2011100227030 A CN 2011100227030A CN 201110022703 A CN201110022703 A CN 201110022703A CN 102603826 A CN102603826 A CN 102603826A
- Authority
- CN
- China
- Prior art keywords
- extracting
- bugle
- acetyl
- crust
- organic solvent
- 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.)
- Pending
Links
Images
Landscapes
- Saccharide Compounds (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method for extracting 8-acetylharpagide from a decumbent bugle herb plant. An extracting method of which the patent application number is 200510085017 is used for extracting by taking an extract obtained from the decumbent bugle herb plant as a raw material. The method comprises the following steps of: dissolving a raw material into a methanol or ethanol solvent, filtering, and drying a filtrate to obtain a crude extract; and dissolving the crude extract into a specific organic solvent, filtering, recovering a part of the solvent, standing for a certain period of time, precipitating a crystal out, filtering, and repeatedly purifying a precipitate to obtain 8-acetylharpagide of which the purity is over 90 percent. Due to the adoption of the method, the purity of the 8-acetylharpagide serving as a main active ingredient is improved on the basis of an original patent; and the method has the advantages of stable process, high repeatability, easiness for operating and suitability for industrial production.
Description
Technical field
The present invention relates to tcm-pharmaceutical technology field, especially a kind of Chemistry for Chinese Traditional Medicine process for extracting.
Background technology
The Labiatae Herba ajugae ciliatae (Herba Ajugae Ajuga ciliata Bge.) belongs to the Ajuga plant whole world has kind more than 40 approximately, is distributed widely in Europe, area, temperate zone, inferior continent, and area, the Near East distributes more concentrated; China has 18 kinds, and great majority are distributed on the south the Qinling Mountains, Anhui, Jiangsu, Jiangxi, Fujian, Zhejiang, Hubei, Hunan, Sichuan, Tibet etc.This genus has many kinds as among the people medicinal; The medicinal beginning of Herba ajugae ciliatae (Herba Ajugae Ajuga ciliata Bge.) is stated from supplement to the Herbal, and its former plant comprises various plants such as ajuga decumbens A.decumbens, japanese bugle herb A.nipponensis, white luxuriant Herba ajugae ciliatae (Herba Ajugae Ajuga ciliata Bge.) A.luputina, Herba Ajugae Lupulinae A juga lupulina var.m ajor, Herba ajugae ciliatae (Herba Ajugae Ajuga ciliata Bge.) A.ciliata.Herb is medicinal, has the effect of clearing heat and detoxicating, expelling phlegm for arresting cough, cooling blood for hemostasis; Can be used for treating diseases such as cough due to lung-heat, swelling and pain in the throat, the swollen sore furuncle of carbuncle.The southern diseases such as ulcer treatment sore, pinkeye, acute mastitis, nosebleed epistaxis, pharyngolaryngitis, gastroenteritis, acute conjunctivitis, scald, dog bite, venom and traumatic hemorrhage that Herba ajugae ciliatae (Herba Ajugae Ajuga ciliata Bge.) is used to treat among the people of China.Modern study finds that this platymiscium has vasoconstriction, pharmacologically active such as antibacterial, antitumor.Evident in efficacy in treatment hysteromyoma and gynecological inflammation, can obviously improve clinical symptom such as hyperhematosis, more obvious to the restraining effect of early stage myomata, the most remarkable to the intramural myoma curative effect especially.
The document and inventor test of pesticide effectiveness result in earlier stage shows that all the basic substance of treatment hysteromyoma is the iridoid glycoside constituents in the Herba ajugae ciliatae (Herba Ajugae Ajuga ciliata Bge.).And 8-acetyl Kazakhstan crust glycosides accounts for 70% of total iridoid glycoside constituents in the iridoid glycoside constituents; Therefore; It is main onset composition that 8-acetyl is breathed out crust glycosides monomer; Test of pesticide effectiveness result also proves the effect that 8-acetyl Kazakhstan crust glycosides has tangible Chinese People's Anti-Japanese Military and Political College mouse hysteromyoma really, and effects such as anti-inflammatory, pain relieving are remarkable.
The inventor once disclosed Herba ajugae ciliatae (Herba Ajugae Ajuga ciliata Bge.) extract (application number 200510085017); But wherein the extract of indication is 50-99% for extract, the purity of breathing out crust glycosides and Ha Ba glycosides total with 8-acetyl; Exist technology unstable, contain non-main onset composition, dose problem rambunctious.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method that 8-acetyl is breathed out the crust glycosides of from bugle, effectively extracting, and makes that its purity is higher, technology is more stable.
For solving the problems of the technologies described above, technical scheme of the present invention is:
8-acetyl is breathed out the process for extracting of crust glycosides in the bugle, and the extract that with number of patent application is process for extracting gained from bugle of 200510085017 is that raw material carries out purifying and extracts, and may further comprise the steps:
(1) raw material is dissolved in ethanol or the methanol solvate, filters, filtrate decompression is recycled to does not have the alcohol flavor, gets crude extract after the drying.
(2) step (1) gained crude extract is dissolved in the organic solvent that polarity is 3.0-7.0, filters, decompression and solvent recovery stops after having small amount of crystalline to separate out, and leaves standstill, and no longer separates out to crystallization, and crystallization is separated with mother liquor.
(3) xln with step (2) gained dissolves in the organic solvent again, and step (2) repeats 2-5 time, obtains 8-acetyl and breathes out crust glycosidal crystalline body.
In the said extracted method, the bugle of indication comprises that bugle such as gold grey little grass, japanese bugle herb and other contain the plant that 8-acetyl is breathed out the crust glycosides, and used part is this plant herb.
Preferably, in the said extracted method, concentration of ethanol is that 70-95%, methyl alcohol are 70-100% in the said step (1), and consumption is 5-20 times (ml/g) of raw material.
Preferably, in the said extracted method, the organic solvent of said step (2) is one of following: methyl alcohol, ethanol, absolute ethyl alcohol, acetone, propyl carbinol, Virahol, butanone, ETHYLE ACETATE, trichloromethane.
Preferably, in the said extracted method, the consumption of the middle organic solvent of said step (2) is 20-100 a times of crude extract.
Preferably, in the said extracted method, said step can add gac in (2), and consumption is 0.5-2 a times of crude extract.
Preferably, in the said extracted method, 8-acetyl is breathed out the medicine that crust glycosidal crystalline body is used to prepare treatment hysteromyoma or gynecological inflammation in the said step (3).
The invention has the beneficial effects as follows:
8-acetyl is breathed out the process for extracting of crust glycosides in the said bugle, has overcome that former invented technology is unstable, the purity fluctuation is big, has contained the non-main onset shortcoming that becomes to grade; On its basis, carry out purifying and extract, the purity that makes 8-acetyl breathe out the crust glycosides reaches more than 90%, process stabilizing, good reproducibility, simple to operate, be suitable for suitability for industrialized production.
Description of drawings
Fig. 1 breathes out the general structure of crust glycosides for 8-O-acetyl
Embodiment
(1) from the herb of the grey little grass of bugle gold, with application number be 200510085017 process for extracting extract obtained be raw material.With raw material 50g, be dissolved in 95% ethanol 1000ml, to filter, filtrate decompression is recycled to does not have the alcohol flavor, the dry runic thing 40g that gets.
(2) the gained crude extract adds the 40g gac, and mixing adds methyl alcohol 800ml and refluxes each 0.5 hour 2 times; Filtering liquid medicine, the reclaim under reduced pressure partial solvent stops after having small amount of crystalline to separate out; Stand at low temperature to crystallization is no longer separated out, and crystallization is separated with mother liquor, gets crystallization 18.2g.
(3) crystallization is dissolved in the 400ml absolute ethyl alcohol, the reclaim under reduced pressure partial solvent stops after having small amount of crystalline to separate out, and stand at low temperature to crystallization is no longer separated out, and crystallization is separated with mother liquor, gets 8-acetyl and breathes out crust glycosides 12.5g, and extraction yield is 25%, and purity is 97%.
(1) from the herb of bugle japanese bugle herb, with application number be 200510085017 process for extracting extract obtained be raw material.With raw material 50g, be dissolved in 85% ethanol 1200ml, to filter, filtrate decompression is recycled to does not have the alcohol flavor, the dry runic thing 42g that gets.
(2) the gained crude extract adds the 21g gac, and mixing adds acetone 3000ml and refluxed 1 hour, filtering liquid medicine, and the reclaim under reduced pressure partial solvent stops after having small amount of crystalline to separate out, and stand at low temperature to crystallization is no longer separated out, and crystallization is separated with mother liquor, gets crystallization 17.6g.
(3) crystallization is added the 1000ml dissolve with methanol, the reclaim under reduced pressure partial solvent stops after having small amount of crystalline to separate out, and stand at low temperature to crystallization is no longer separated out, and crystallization is separated with mother liquor, gets 8-acetyl and breathes out crust glycosides 15.4g.
(4) repeating step is (3) 2 times, gets 8-acetyl and breathes out crust glycosides 13.6g, extraction yield 27.2%, purity 99%.
(1) from the herb of the grey little grass of bugle gold, with application number be 200510085017 process for extracting extract obtained be raw material.With raw material 50g, be dissolved in 100% methyl alcohol 250ml, to filter, filtrate decompression is recycled to does not have the alcohol flavor, the dry runic thing 36g that gets.
(2) the gained crude extract adds ETHYLE ACETATE 5000ml backflow 2 times, and each 0.5 hour, filtering liquid medicine, the reclaim under reduced pressure partial solvent stops after having small amount of crystalline to separate out, and stand at low temperature to crystallization is no longer separated out, and crystallization is separated with mother liquor, gets crystallization 14.2g.
(3) crystallization is dissolved in 1200ml acetone, the reclaim under reduced pressure partial solvent stops after having small amount of crystalline to separate out, and stand at low temperature to crystallization is no longer separated out, and crystallization is separated with mother liquor, gets 8-acetyl and breathes out crust glycosides 11.5g.
(4) repeating step is (3) 5 times, gets 8-acetyl and breathes out crust glycosides 8.5g, extraction yield 17%, purity 98%.
Claims (8)
1. 8-acetyl is breathed out the process for extracting of crust glycosides in the bugle, and the extract that with number of patent application is process for extracting gained from bugle of 200510085017 is that raw material carries out purifying and extracts, and it is characterized in that, may further comprise the steps:
(1) raw material is dissolved in ethanol or the methanol solvate, filters, filtrate decompression is recycled to does not have the alcohol flavor, gets crude extract after the drying.
(2) step (1) gained crude extract is dissolved in the organic solvent that polarity is 3.0-7.0, filters, decompression and solvent recovery stops after having small amount of crystalline to separate out, and leaves standstill, and no longer separates out to crystallization, and crystallization is separated with mother liquor.
(3) xln with step (2) gained dissolves in the organic solvent again, and step (2) repeats 2-5 time, obtains 8-acetyl and breathes out crust glycosidal crystalline body.
2. the process for extracting of bugle according to claim 1; It is characterized in that; Said bugle comprises that bugle such as gold grey little grass, japanese bugle herb and other contain the plant that 8-acetyl is breathed out the crust glycosides, and used part is this plant herb.
3. the process for extracting of bugle according to claim 1 is characterized in that, concentration of ethanol is that 70-95%, methyl alcohol are 70-100% in the said step (1), and consumption is 5-20 times (ml/g) of raw material.
4. the process for extracting of bugle according to claim 1; It is characterized in that the organic solvent of said step (2) or (3) is one of following: methyl alcohol, ethanol, absolute ethyl alcohol, acetone, propyl carbinol, Virahol, butanone, ETHYLE ACETATE, trichloromethane.
5. the process for extracting of bugle according to claim 1 is characterized in that, said step (2) is different with (3) used organic solvent.
6. according to the process for extracting of claim 1 or 4 described bugles, it is characterized in that the consumption of the middle organic solvent in said step (2) or (3) is 20-100 a times of crude extract.
7. the process for extracting of bugle according to claim 1 is characterized in that, said step can add gac in (2), and consumption is 0.5-2 a times of crude extract.
8. the process for extracting of bugle according to claim 1 is characterized in that, 8-acetyl is breathed out the medicine that crust glycosidal crystalline body is used to prepare treatment hysteromyoma or gynecological inflammation in the said step (3).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100227030A CN102603826A (en) | 2011-01-20 | 2011-01-20 | Method for extracting 8-acetylharpagide from decumbent bugle herb plant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100227030A CN102603826A (en) | 2011-01-20 | 2011-01-20 | Method for extracting 8-acetylharpagide from decumbent bugle herb plant |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102603826A true CN102603826A (en) | 2012-07-25 |
Family
ID=46521647
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011100227030A Pending CN102603826A (en) | 2011-01-20 | 2011-01-20 | Method for extracting 8-acetylharpagide from decumbent bugle herb plant |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102603826A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104606284A (en) * | 2013-11-05 | 2015-05-13 | 北京康辰药业有限公司 | New uses of Ajuga ciliata Bunge extract |
| CN110812386A (en) * | 2019-12-20 | 2020-02-21 | 佛山科学技术学院 | Anti-inflammatory effective part of small incised wound grass as well as preparation method and application thereof |
| CN111973652A (en) * | 2019-05-23 | 2020-11-24 | 法玛科技顾问股份有限公司 | Method for treating cell aging |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999058155A1 (en) * | 1998-05-14 | 1999-11-18 | The Salk Institute For Biological Studies | Formulations useful for modulating expression of exogenous genes in mammalian systems, and products related thereto |
| CN1899367A (en) * | 2005-07-19 | 2007-01-24 | 中国中医研究院中药研究所 | Carpet bugle extract, its preparing method, use and composite preparation |
| CN101260131A (en) * | 2008-04-19 | 2008-09-10 | 吉首大学 | Method for extracting iridoid active site and monomer from eucommia bark |
-
2011
- 2011-01-20 CN CN2011100227030A patent/CN102603826A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999058155A1 (en) * | 1998-05-14 | 1999-11-18 | The Salk Institute For Biological Studies | Formulations useful for modulating expression of exogenous genes in mammalian systems, and products related thereto |
| CN1899367A (en) * | 2005-07-19 | 2007-01-24 | 中国中医研究院中药研究所 | Carpet bugle extract, its preparing method, use and composite preparation |
| CN101260131A (en) * | 2008-04-19 | 2008-09-10 | 吉首大学 | Method for extracting iridoid active site and monomer from eucommia bark |
Non-Patent Citations (4)
| Title |
|---|
| 《Khimiya Prirodnykh Soedinenii》 19681231 V. I. Litvinenko，等 "Iridoids of Betonica foliosa" 第319页 1-8 第4卷, 第5期 * |
| 《中国实验方剂学杂志》 20091130 王锦玉，等 "RP-HPLC法同时测定筋骨草药材中哈巴苷和乙酰哈巴苷含量" 第26-28页 1-8 第15卷, 第11期 * |
| V. I. LITVINENKO，等: ""Iridoids of Betonica foliosa"", 《KHIMIYA PRIRODNYKH SOEDINENII》 * |
| 王锦玉，等: ""RP-HPLC法同时测定筋骨草药材中哈巴苷和乙酰哈巴苷含量"", 《中国实验方剂学杂志》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104606284A (en) * | 2013-11-05 | 2015-05-13 | 北京康辰药业有限公司 | New uses of Ajuga ciliata Bunge extract |
| CN111973652A (en) * | 2019-05-23 | 2020-11-24 | 法玛科技顾问股份有限公司 | Method for treating cell aging |
| CN110812386A (en) * | 2019-12-20 | 2020-02-21 | 佛山科学技术学院 | Anti-inflammatory effective part of small incised wound grass as well as preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103204839B (en) | Synchronous preparation method of effective ingredient of licorice | |
| CN103408564B (en) | The extraction and purification process of eurycomanone in Tongkat Ali plant | |
| CN103772473A (en) | Vacuum pulse type method of extracting and purifying ursolic acid of rosemary | |
| CN101040950B (en) | Method of preparing compound Houttuynia cordata dropping pills | |
| CN104873558A (en) | Preparation method of black ginseng with high-content ginsenoside | |
| CN102304501A (en) | Complex enzyme preparation and application and method thereof for extracting plant polysaccharides by using same | |
| CN104292352A (en) | Method for extracting and separating eucommia ulmoides flavor powder, eucommia ulmoides oliv polysaccharides and eucommea rubber through coproduction | |
| CA2486378A1 (en) | Preparation and application of total salvianolic acid | |
| CN102178730B (en) | Platycarya strobilacea sieb infructescence polyphenols extract as well as extracting method and application thereof | |
| CN101538296A (en) | Active ingredients of camptosorus sibiricus, and extraction method and use of same | |
| CN102603826A (en) | Method for extracting 8-acetylharpagide from decumbent bugle herb plant | |
| CN102302672B (en) | Honeysuckle flower buccal tablets and preparation method thereof | |
| CN100333753C (en) | Extraction technology of plant total alkaloid extract having anti tumour action and its preparation | |
| CN101953883A (en) | Chinese medicinal granules for treating calculosis and preparation method thereof | |
| CN103054917A (en) | Application for freeze-dried purslane in medicine preparation | |
| CN102895303A (en) | Resin purification method for extracting and separating total flavone of cyclocarya paliurus | |
| CN102336803A (en) | Purification and preparation method for aescin extract | |
| CN102241574B (en) | Method for preparing high-purity protocatechualdehyde from salvia miltiorrhiza | |
| CN103145703A (en) | Process technique to prepare rotundine based on different plants | |
| CN105641014B (en) | Nandina total alkaloid extract and its application in preparing treatment pharyngitis drug | |
| CN108685964B (en) | Application of gerbera piloselloides extract and preparation method of active ingredients of gerbera piloselloides extract | |
| CN103070893A (en) | Medicine prepared by purslane and used for treating senile dementia | |
| CN102391232B (en) | The method of Liquiritigenin is extracted from Radix Glycyrrhizae | |
| CN102718811A (en) | Preparation method of stilbene glycoside in polygonum cuspidatum | |
| CN101974001A (en) | Process for extracting pure liriodenine from Chinese tuliptree barks |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120725 |