CN101962385A - Method for preparing bergeninum - Google Patents
Method for preparing bergeninum Download PDFInfo
- Publication number
- CN101962385A CN101962385A CN2010105108207A CN201010510820A CN101962385A CN 101962385 A CN101962385 A CN 101962385A CN 2010105108207 A CN2010105108207 A CN 2010105108207A CN 201010510820 A CN201010510820 A CN 201010510820A CN 101962385 A CN101962385 A CN 101962385A
- Authority
- CN
- China
- Prior art keywords
- bergeninum
- preparation
- adds
- macroporous resin
- described step
- 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
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Nitrogen And Oxygen Or Sulfur-Condensed Heterocyclic Ring Systems (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention provides a method for preparing bergeninum. The method comprises the following steps of: crushing saxifragaceae plants such as purple bergenia, astilbe chinensis or Japanese ardisia serving as raw materials; adding 15 to 20 times the amount of saturated limewater for percolating and extracting; filtering and adding an ultrafiltration membrane into extracting solution for performing ultrafiltration; adding a proper amount of water for dialyzing; collecting permeate liquid; regulating the pH of the permeate liquid to be between 2 and 3; filtering precipitate out; refluxing and dissolving the precipitate by using hot water; adding macroporous resin for performing column adsorption; eluting by using the solution of limewater with the pH of between 8 and 10; regulating the pH of eluent to be between 3 and 5; filtering crystals; refluxing and dissolving a filtrate with 99 percent ethanol; and performing recrystallization and vacuum-drying to obtain a product. The method for preparing the bergeninum has simple process operation and low energy cost, meets the requirements on energy-saving and emission-reduction, and is suitable for industrialization.
Description
Technical field:
The present invention relates to a kind of preparation method of Bergeninum, particularly relate to the method that a kind of membrane sepn and macroporous resin prepare Bergeninum.
Background technology:
Bergeninum is vakerin again, the needle crystal of white loose or crystalline powder; Odorless, bitter; Meet light or hot gradual change look.In methyl alcohol, dissolve slightly soluble in water or ethanol.Molecular formula: C14H16O9; Molecular weight: 328.27.
Bergeninum has kobadrin, is used for the chronic bronchitis treatment.Now the Bergeninum extract lists that " Chinese pharmacopoeia also has patent medicine Bergeninum sheet in.
Bergeninum mainly extracts from brave otology phytogenic rock Chinese cabbage, Herba astilbes chinensis and Japanese Ardisia Herb.The Bergeninum extraction process is more, and organic reagent or water refluxing extraction are arranged, and the acid-base precipitation method also has the extraction of resin method and supercritical CO 2, the technology comparative maturity." Bergeninum extraction process preparation and the quality standard research summary " that Sun Min etc. deliver, document has outlined current technology in detail.Also have people such as Hu Wenjie to adopt macroporous resin to separate Bergeninum in addition, people such as Gao Jie adopt supercritical CO 2 extraction Bergeninum.Patent documentation is as " process for quickly and demicontinuously extracting bergenin ", the method of patent disclosure be of the present invention fast semicontinuous be extracted as the medicinal powder after the pulverization process is positioned over add 0.5-3 solvent doubly in the encloses container, behind 25-50 ℃ of infiltration 0.5-2h, with 25-50 ℃ solvent, with 6ml/kgmin
-1～35ml/kgmin
-1The leaching velocity lixiviate; Reconcentration, refining, promptly get the Bergeninum finished product.
As mentioned above, there are problems such as energy consumption height or organic reagent consumption height or industrialization degree are low in existing technology.
Summary of the invention:
The present invention wants the technical solution problem to provide the preparation method of a kind of less energy-consumption, Bergeninum simple to operate.
The objective of the invention is to realize by following technical solution:
A kind of preparation method of Bergeninum is characterized in that comprising following steps:
1) get raw material pulverizing, add 15-20 and doubly measure the saturated limewater diacolation and extract, filter extracting solution;
2) said extracted liquid adds the ultra-filtration membrane ultrafiltration, adds the suitable quantity of water dialysis, collects and sees through liquid;
3) the above-mentioned liquid that sees through is regulated the ph2-3 precipitation, leaches throw out, and throw out hot water refluxes and dissolves, and adds macroporous resin adsorption, and the lime aqueous solution wash-out of ph8-10 is collected elutriant;
4) above-mentioned elutriant is regulated ph3-5 and is placed crystallization, and crystallisate leaches, and uses 99% alcohol reflux dissolving-recrystallization again, and vacuum-drying gets product.
A kind of in the optional saxifragaceae plant Rhizome or herb of Purple Bergenia of the raw material of described step 1), Herba astilbes chinensis or the Japanese Ardisia Herb.
Described step 2) ultra-filtration membrane is the tubular type composite hyperfiltration membrane of molecular weight cut-off 3000-6000 in.
A kind of among the optional AB-8 of described step 3) macroporous resin model, ADS-8, HZ818 and the ADS-17.
Present method positively effect is: adopting the liming diacolation, is that open loop under alkaline condition becomes water-soluble salt according to Bergeninum, has also reduced the stripping of tannin simultaneously, macromolecular substance is removed in the ultra-filtration membrane ultrafiltration again, closed loop precipitation under acidic conditions, macroporous resin separation, recrystallization are gone up in dissolving again.Whole process flow has adopted the less energy-consumption method, reduces acid-alkali treatment number of times and organic reagent crystallization number of times, and organic reagent has only been used ethanol, and production cost is lower, and products obtained therefrom meets the medicine requirement.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment:
Embodiment:
Embodiment 1:
Get the Rhizome or herb of Purple Bergenia raw material pulverizing, get 10kg, adding 20 times of amount saturated limewater diacolations extracted 20 hours, filter, extracting solution adds the tubular type composite hyperfiltration membrane system ultrafiltration of molecular weight cut-off 3000-6000, adds the suitable quantity of water dialysis, sees through liquid hydrochloric acid and regulates the ph2 precipitation, leach throw out, throw out hot water refluxes and dissolves, after the absorption of adding AB-8 macroporous resin column, with the lime aqueous solution wash-out of ph8, collect elutriant and regulate hydrochloric acid ph4 placement crystallization, crystallisate leaches, and uses 99% alcohol reflux dissolving-recrystallization again, and vacuum-drying gets the white, needle-shaped crystals Bergeninum, content 98.6%, yield 3.5%.
Embodiment 2:
Get the Herba astilbes chinensis raw material pulverizing, get 10kg, adding 15 times of amount saturated limewater diacolations extracted 24 hours, filter, extracting solution adds the tubular type composite hyperfiltration membrane system ultrafiltration of molecular weight cut-off 3000-6000, adds the suitable quantity of water dialysis, sees through molten sulfur acid and regulates the ph3 precipitation, leach throw out, throw out hot water refluxes and dissolves, after the absorption of adding ADS-8 macroporous resin column, with the lime aqueous solution wash-out of ph10, collect elutriant and regulate sulfuric acid ph3 placement crystallization, crystallisate leaches, and uses 99% alcohol reflux dissolving-recrystallization again, and vacuum-drying gets the white, needle-shaped crystals Bergeninum, content 98.2%, yield 3.0%.
Embodiment 3:
Get the Japanese Ardisia Herb raw material pulverizing, get 10kg, adding 20 times of amount saturated limewater diacolations extracted 20 hours, filter, extracting solution adds the tubular type composite hyperfiltration membrane system ultrafiltration of molecular weight cut-off 3000-6000, adds the suitable quantity of water dialysis, sees through liquid hydrochloric acid and regulates the ph3 precipitation, leach throw out, throw out hot water refluxes and dissolves, after the absorption of adding HZ818 macroporous resin column, and the lime aqueous solution wash-out of ph9, collect elutriant and regulate ph5 placement crystallization, crystallisate leaches, and uses 99% alcohol reflux dissolving-recrystallization again, and vacuum-drying gets the white, needle-shaped crystals Bergeninum, content 97.5%, yield 2.8%.
Claims (4)
1. the preparation method of a Bergeninum is characterized in that comprising following steps:
1) get raw material pulverizing, add 15-20 and doubly measure the saturated limewater diacolation and extract, filter extracting solution;
2) said extracted liquid adds the ultra-filtration membrane ultrafiltration, adds the suitable quantity of water dialysis, collects and sees through liquid;
3) the above-mentioned liquid that sees through is regulated the ph2-3 precipitation, leaches throw out, and throw out hot water refluxes and dissolves, and adds macroporous resin adsorption, and the lime aqueous solution wash-out of ph8-10 is collected elutriant;
4) above-mentioned elutriant is regulated ph3-5 and is placed crystallization, and crystallisate leaches, and uses 99% alcohol reflux dissolving-recrystallization again, and vacuum-drying gets product.
2. according to claim 1 from the preparation method of Bergeninum, it is characterized in that a kind of in the optional saxifragaceae plant Rhizome or herb of Purple Bergenia of raw material, Herba astilbes chinensis or the Japanese Ardisia Herb of described step 1).
3. according to claim 1 from the preparation method of Bergeninum, it is characterized in that described step 2) in ultra-filtration membrane be the tubular type composite hyperfiltration membrane of molecular weight cut-off 3000-6000.
4. according to claim 1 from the preparation method of Bergeninum, it is characterized in that in the described step 3) a kind of among the optional AB-8 of macroporous resin model, ADS-8, HZ818 and the ADS-17.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105108207A CN101962385A (en) | 2010-10-19 | 2010-10-19 | Method for preparing bergeninum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105108207A CN101962385A (en) | 2010-10-19 | 2010-10-19 | Method for preparing bergeninum |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101962385A true CN101962385A (en) | 2011-02-02 |
Family
ID=43515448
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010105108207A Pending CN101962385A (en) | 2010-10-19 | 2010-10-19 | Method for preparing bergeninum |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101962385A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105851076A (en) * | 2016-04-29 | 2016-08-17 | 山东胜伟园林科技有限公司 | Biopesticide containing Bacillus sphaericus and used for preventing and treating soybean diseases and pests |
| CN106749298A (en) * | 2016-11-18 | 2017-05-31 | 文县嘉诚农副产品有限公司 | A kind of Bergenin is extracted and process for purification |
| CN108840892A (en) * | 2018-08-09 | 2018-11-20 | 湖南农业大学 | A method of extracting quercitrin and Bergenin from ardisia japonica |
| WO2021093632A1 (en) * | 2019-11-15 | 2021-05-20 | 杭州百芮生物科技有限公司 | Active essence compounded with postbiotics and preparation method |
-
2010
- 2010-10-19 CN CN2010105108207A patent/CN101962385A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105851076A (en) * | 2016-04-29 | 2016-08-17 | 山东胜伟园林科技有限公司 | Biopesticide containing Bacillus sphaericus and used for preventing and treating soybean diseases and pests |
| CN106749298A (en) * | 2016-11-18 | 2017-05-31 | 文县嘉诚农副产品有限公司 | A kind of Bergenin is extracted and process for purification |
| CN106749298B (en) * | 2016-11-18 | 2019-03-29 | 文县嘉诚农副产品有限公司 | A kind of Bergenin extracts and refining methd |
| CN108840892A (en) * | 2018-08-09 | 2018-11-20 | 湖南农业大学 | A method of extracting quercitrin and Bergenin from ardisia japonica |
| CN108840892B (en) * | 2018-08-09 | 2021-07-09 | 湖南农业大学 | Method for extracting quercetin and bergenin from Japanese ardisia |
| WO2021093632A1 (en) * | 2019-11-15 | 2021-05-20 | 杭州百芮生物科技有限公司 | Active essence compounded with postbiotics and preparation method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101016328B (en) | Method of separating and purifying ursolic acid and oleanolic acid | |
| CN102101840B (en) | Method for extracting and separating high-purity 1-Deoxynojirimycin from folium mori | |
| CN102399187A (en) | Preparation method of sinomenine | |
| CN108409640A (en) | A kind of method of purification of arecaline | |
| CN105949185B (en) | Kwangsi stephania root prepares rotundin hydrochloride method | |
| CN101962385A (en) | Method for preparing bergeninum | |
| CN103923139A (en) | Method for extracting rutin from sophora flower buds | |
| CN102234245A (en) | Method for preparing sulforaphane | |
| CN102643315B (en) | Method for purifying phlorizin from apple velamen | |
| CN103664669A (en) | Process method for preparing high-purity levodopa | |
| CN109369733A (en) | A method of extracting a variety of flavone compounds simultaneously from leaf of Radix Et Rhizoma Fagopyri Tatarici | |
| CN101759731B (en) | Extraction method of linseed gum and secoisolariciresin-ol diglucoside | |
| CN100539859C (en) | From tealeaves, extract the method for Tea Polyphenols | |
| CN102040611A (en) | Method for extracting mulberry root ketone C | |
| CN101973983A (en) | Method for extracting orientins from Chinese globeflower flowers | |
| CN104262421B (en) | The technique extracting salicoside from Populus euphratica fallen leaves | |
| CN103102270A (en) | Preparation method of chlorogenic acid | |
| CN105646620B (en) | The preparation method of fleabane flower A prime | |
| CN104231011A (en) | Preparation method of verbascoside | |
| CN105732743B (en) | The method that extraction prepares high-purity kaempferia galamga glycosides from burmann cinnamon leaf | |
| CN104926766A (en) | Method for synchronous extraction of quercetin and nuciferine from lotus leaves | |
| CN102697838A (en) | Method for extracting and separating flavone enrichment substance, saponin enrichment substance and polysaccharide from astragalus simultaneously | |
| CN105250391B (en) | A kind of preparation method of slenderstalk dicranostigma herb alkaloid valid target | |
| CN102232995A (en) | Preparation method of total flavonoids in medicago sativa L. | |
| CN102659873A (en) | Method for extracting nicotifiorin from nymphaea candida presl |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20110202 |