CN102895303A - Resin purification method for extracting and separating total flavone of cyclocarya paliurus - Google Patents
Resin purification method for extracting and separating total flavone of cyclocarya paliurus Download PDFInfo
- Publication number
- CN102895303A CN102895303A CN2012104438158A CN201210443815A CN102895303A CN 102895303 A CN102895303 A CN 102895303A CN 2012104438158 A CN2012104438158 A CN 2012104438158A CN 201210443815 A CN201210443815 A CN 201210443815A CN 102895303 A CN102895303 A CN 102895303A
- Authority
- CN
- China
- Prior art keywords
- cyclocarya paliurus
- paliurus iljinskaja
- total flavones
- ethanol
- resin
- 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
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to a method for purifying total flavone of cyclocarya paliurus, belonging to the field of traditional Chinese medicine. The method comprises the technical steps of: reflowing and extracting medicinal materials by ethanol, absorbing by macroporous resin and washing by water, abandoning washing liquor, continuously washing by alkali and water, collecting alkali washing liquor and water continuous washing liquor, absorbing by macroporous resin after the pH is adjusted with acid, eluting the ethanol with a certain concentration, collecting ethanol eluant, concentrating, and drying to obtain the total flavone extractive of the cyclocarya paliurus. The total flavone of the cyclocarya paliurus is produced after the method is adopted, so that the method is simple in technology and low in energy consumption, the macroporous resin and the ethanol can be repeatedly used, and the obtained product is high in purity. The technology is suitable for the industrial production.
Description
Technical field
The present invention relates to the medicine separation technical field, particularly a kind of extraction and separation process that utilizes macroporous adsorbent resin to prepare high-purity Cyclocarya paliurus Iljinskaja total flavones.
Background technology
Cyclocarya paliurus Iljinskaja has another name called blue or green money Lee (Jiangxi), Boehmeria longispica Steud. willow (Sichuan), Folium hydrangeae strigosae tree (Guizhou), a string money (Hubei), is Dicotyledoneae Juglandaceae cyclocarya plant.Belong to national second class protection seeds.Be distributed widely in mountain area, trench or the Limestone Mountain of the height above sea level 420～2500m such as Jiangxi, Zhejiang, Jiangsu, Anhui, Fujian, Taiwan, Hubei, Sichuan, Guizhou, Yunnan." national Chinese herbal medicine name mirror " record: the Cyclocarya paliurus Iljinskaja bark, leaf, root has killing parasites for relieving itching, the effect that anti-inflammatory analgetic dispels the wind.The quench one's thirst effect of detoxifcation of " Chinese medicine resource will will " record, the heat clearing away of leaf of Cyclocarya paliurus Iljinskaja tool.Tcm clinical practice is used for the treatment of diabetes, because it has pharmacological action obviously blood sugar lowering, fat reducing fat and glucose in urine.The modern science experiment finds that leaf of Cyclocarya paliurus Iljinskaja contains the multiple important active ingredient such as flavone, polysaccharide, triterpenoid, saponin, steroidal compounds, alkaloid, organic acid, also detects simultaneously aminoacid, vitamin, germanium, selenium, chromium, vanadium, zinc, ferrum, the trace element of the multiple preciousness such as calcium.It has blood sugar lowering, blood fat reducing, blood pressure lowering, antioxidation, anti-aging, strengthen the effect such as immunity, have broad application prospects.
At present the extracting method of Cyclocarya paliurus Iljinskaja effective ingredient has caused extensive concern, and Chinese patent application number is 200810073472.4 to disclose a kind of " extracting the method for polysaccharide and effective ingredient from Cyclocarya paliurus Iljinskaja ", adopts membrane separation process to extract preparation Cyclocarya paliurus Iljinskaja polysaccharide.Chinese patent application number is 200810061167.3 to disclose " a kind of preparation method of natural plant extracts ", adopts alcohol extraction, concentrating under reduced pressure to prepare Cyclocarya paliurus Iljinskaja crude product extract.Chinese patent application numbers 201010138672.0 discloses a kind of " extraction process of blood sugar reducing active saponin from cyclocarya paliurus ", and the methods such as alcohol extraction, petroleum ether extraction, macroporous resin separation are extracted the technique of Cyclocarya paliurus Iljinskaja saponin.Existing patent does not relate to the preparation technology of high-purity Cyclocarya paliurus Iljinskaja total flavones.
Summary of the invention
The object of the present invention is to provide a kind of macroporous resin isolation and purification method of Cyclocarya paliurus Iljinskaja total flavones, be with the Cyclocarya paliurus Iljinskaja extracting solution through resin upper prop, eluting, collection eluent, concentrated, dry, obtain highly purified Cyclocarya paliurus Iljinskaja total flavones.
A kind of resin purification method of separating the Cyclocarya paliurus Iljinskaja total flavones of extracting provided by the invention, realize by following steps:
(1) Cyclocarya paliurus Iljinskaja is pulverized, with 8～12 times of certain density alcohol reflux 2～4 hours, extracted merge extractive liquid, 2～3 times.
(2) with the extracting solution Recycled ethanol, be concentrated into an amount of volume, add macroporous resin adsorption, use first the purified water eluting of 2～5 times of resin volumes, use again the aqueous slkali eluting of 1～3 times of resin volume, use again 2～5 times of purified water eluting, collect alkali and water elution liquid.
(3) with behind the alkali in the step (2) and water elution liquid acid adding accent Ph to 2～5, upper macroporous resin adsorption is used 50%～80% ethanol elution again, collects alcohol eluen.
(4) with the alcohol eluen concentrating under reduced pressure, drying had both got the Cyclocarya paliurus Iljinskaja total flavones.
Concentration of alcohol in the step (1) is 50%～90%
The optional sodium carbonate of alkali in the step (2), calcium carbonate, sodium bicarbonate, calcium bicarbonate.The macroporous resin model can be among AB-8, D101, HPD100, HPD400, HPD427, HPD600, HPD722, the HPD826 a kind of, medical material weight: the resin volume is 1: 1～1: 3.
Sour optional hydrochloric acid, phosphoric acid or sulphuric acid in the step (3) a kind of.The macroporous resin model can be among AB-8, D101, HPD100, HPD400, HPD427, HPD600, HPD722, the HPD826 a kind of.Medical material weight: the resin volume is 1: 0.5～1: 1.
The present invention has the following advantages:
1, Cyclocarya paliurus Iljinskaja total flavonoid resin purification process provided by the invention is easy and simple to handle, quick;
2, selected macroporous resin has that adsorbance is large, resolution factor is large, renewable reusing;
3, with purification Cyclocarya paliurus Iljinskaja of the present invention, the rate of transform of its total flavones reaches more than 90%, and the Cyclocarya paliurus Iljinskaja general flavone content reaches more than 75%.
Description of drawings
Purifying process flow chart for the Cyclocarya paliurus Iljinskaja total flavones.
The specific embodiment
Embodiment 1
With Cyclocarya paliurus Iljinskaja medical material 1kg, pulverize, measure 70% alcohol reflux 2 times with 10 times, each 3 hours, merge extractive liquid,, Recycled ethanol, and be evaporated to an amount of, the concentrated solution AB-8 macroporous resin adsorption of 1000ml, with the flushing of 5000ml purified water, discard eluent, use again 2% calcium carbonate soln 3000ml eluting, and add that the 3000ml purified water is continuous washes, collect the continuous washing liquid of alkali and water; To continue washing liquid and add hydrochloric acid accent Ph to 4～5, with the HPD600 macroporous resin adsorption of 500ml, use again 80% ethanol 1500ml eluting, collect alcohol eluen, concentrating under reduced pressure, vacuum drying gets Cyclocarya paliurus Iljinskaja total flavones 9.8g, content 78%.
Embodiment 2
With Cyclocarya paliurus Iljinskaja medical material 1kg, pulverize, measure 90% alcohol reflux 2 times with 8 times, each 2.5 hours, merge extractive liquid,, Recycled ethanol, and be evaporated to an amount of, the concentrated solution D101 macroporous resin adsorption of 2000ml, with the flushing of 8000ml purified water, discard eluent, use again 2% sodium carbonate solution 5000ml eluting, and add that the 6000ml purified water is continuous washes, collect the continuous washing liquid of alkali and water; To continue washing liquid and add sulphuric acid accent Ph to 3～4, with the HPD400 macroporous resin adsorption of 1500ml, use again 60% ethanol 2000ml eluting, collect alcohol eluen, concentrating under reduced pressure, vacuum drying gets Cyclocarya paliurus Iljinskaja total flavones 9.1g, content 80%.
Embodiment 3
With Cyclocarya paliurus Iljinskaja medical material 1kg, pulverize, measure 60% alcohol reflux 3 times with 11 times, each 4 hours, merge extractive liquid,, Recycled ethanol, and be evaporated to an amount of, the concentrated solution HPD400 macroporous resin adsorption of 3000ml, with the flushing of 6000ml purified water, discard eluent, use again 3% sodium bicarbonate solution 4500ml eluting, and add that the 6000ml purified water is continuous washes, collect the continuous washing liquid of alkali and water; To continue washing liquid and add hydrochloric acid accent Ph to 2～3, with the HPD427 macroporous resin adsorption of 3000ml, use again 70% ethanol 4500ml eluting, collect alcohol eluen, concentrating under reduced pressure, vacuum drying gets Cyclocarya paliurus Iljinskaja total flavones 8.9g, content 85%.
Embodiment 4
With Cyclocarya paliurus Iljinskaja medical material 1kg, pulverize, measure 50% alcohol reflux 3 times with 12 times, each 4 hours, merge extractive liquid,, Recycled ethanol, and be evaporated to an amount of, the concentrated solution HPD722 macroporous resin adsorption of 1500ml, with the flushing of 45000ml purified water, discard eluent, use again 2% calcium bicarbonate solution 4500ml eluting, and add that the 4500ml purified water is continuous washes, collect the continuous washing liquid of alkali and water; To continue washing liquid and add hydrochloric acid accent Ph to 3～4, with the HPD826 macroporous resin adsorption of 1500ml, use again 50% ethanol 4500ml eluting, collect alcohol eluen, concentrating under reduced pressure, vacuum drying gets Cyclocarya paliurus Iljinskaja total flavones 8.5g, content 88%.
Claims (6)
1. one kind is extracted the resin purification method of separating the Cyclocarya paliurus Iljinskaja total flavones, it is characterized in that comprising following step:
(1) Cyclocarya paliurus Iljinskaja is pulverized, with 8～12 times of certain density alcohol reflux 2～4 hours, extracted merge extractive liquid, 2～3 times;
(2) with the extracting solution Recycled ethanol, be concentrated into an amount of volume, add macroporous resin adsorption, use first the purified water eluting of 2～5 times of resin volumes, use again the aqueous slkali eluting of 1～3 times of resin volume, use again 2～5 times of purified water eluting, collect alkali and water elution liquid;
(3) with behind the alkali in the step (2) and water elution liquid acid adding accent pH to 2～5, upper macroporous resin adsorption is used 50%～80% ethanol elution again, collects alcohol eluen.
2. the method for described purification Cyclocarya paliurus Iljinskaja total flavones according to claim 1 is characterized in that the concentration of ethanol in the step (1) can be 50%～90%.
3. the method for described purification Cyclocarya paliurus Iljinskaja total flavones according to claim 1, what it is characterized in that macroporous resin used in step (2), (3) can be among AB-8, D101, HPD100, HPD400, HPD427, HPD600, HPD722, the HPD826 is a kind of.
4. the method for described purification Cyclocarya paliurus Iljinskaja total flavones according to claim 1 is characterized in that the optional sodium carbonate of alkali, calcium carbonate, sodium bicarbonate, calcium bicarbonate in the step (2).
5. the method for described purification Cyclocarya paliurus Iljinskaja total flavones according to claim 1, it is characterized in that step (2) Chinese crude drug weight: the resin volume is 1: 1～1: 3.
6. the method for described purification Cyclocarya paliurus Iljinskaja total flavones according to claim 1, it is characterized in that step (3) Chinese crude drug weight: the resin volume is 1: 0.5～1: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012104438158A CN102895303A (en) | 2012-11-09 | 2012-11-09 | Resin purification method for extracting and separating total flavone of cyclocarya paliurus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012104438158A CN102895303A (en) | 2012-11-09 | 2012-11-09 | Resin purification method for extracting and separating total flavone of cyclocarya paliurus |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102895303A true CN102895303A (en) | 2013-01-30 |
Family
ID=47567989
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012104438158A Pending CN102895303A (en) | 2012-11-09 | 2012-11-09 | Resin purification method for extracting and separating total flavone of cyclocarya paliurus |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102895303A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103694364A (en) * | 2013-12-10 | 2014-04-02 | 南昌大学 | Method for synchronously extracting, separating and purifying polysaccharides and flavones of cyclocarya paliurus |
| CN104473981A (en) * | 2014-12-04 | 2015-04-01 | 浙江树人大学 | Method for separating and purifying high-purity general flavone in kandelia candel leaves |
| CN109010422A (en) * | 2018-08-29 | 2018-12-18 | 广州医科大学附属第三医院（广州重症孕产妇救治中心、广州柔济医院） | A kind of preparation method and applications of Qingqian Willow leaf general flavone |
| CN110917240A (en) * | 2019-12-11 | 2020-03-27 | 湖南华诚生物资源股份有限公司 | Continuous method for separating multiple effective components from cyclocarya paliurus |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101829187A (en) * | 2010-04-28 | 2010-09-15 | 广西壮族自治区药用植物园 | Preparation method of fruit-flavored cyclocarya paliurus chewable tablets |
-
2012
- 2012-11-09 CN CN2012104438158A patent/CN102895303A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101829187A (en) * | 2010-04-28 | 2010-09-15 | 广西壮族自治区药用植物园 | Preparation method of fruit-flavored cyclocarya paliurus chewable tablets |
Non-Patent Citations (3)
| Title |
|---|
| 吴彩娥等: "青钱柳叶总黄酮大孔树脂纯化工艺", 《农业机械学报》 * |
| 杨武英等: "聚酰胺树脂精制青钱柳黄酮的研究", 《天然产物研究与开发》 * |
| 陈金华等: "青钱柳叶的化学成分分析", 《食品工业科技》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103694364A (en) * | 2013-12-10 | 2014-04-02 | 南昌大学 | Method for synchronously extracting, separating and purifying polysaccharides and flavones of cyclocarya paliurus |
| CN104473981A (en) * | 2014-12-04 | 2015-04-01 | 浙江树人大学 | Method for separating and purifying high-purity general flavone in kandelia candel leaves |
| CN104473981B (en) * | 2014-12-04 | 2017-12-12 | 浙江树人大学 | A kind of isolation and purification method of high-purity autumn eggplant leaf flavonoids |
| CN109010422A (en) * | 2018-08-29 | 2018-12-18 | 广州医科大学附属第三医院（广州重症孕产妇救治中心、广州柔济医院） | A kind of preparation method and applications of Qingqian Willow leaf general flavone |
| CN110917240A (en) * | 2019-12-11 | 2020-03-27 | 湖南华诚生物资源股份有限公司 | Continuous method for separating multiple effective components from cyclocarya paliurus |
| CN110917240B (en) * | 2019-12-11 | 2021-12-24 | 湖南华诚生物资源股份有限公司 | Continuous method for separating multiple effective components from cyclocarya paliurus |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101775056B (en) | Method for extracting, separating and purifying Astragaloside IV from Astragalus mongholicus | |
| CN101940625B (en) | Preparation method and use of extract | |
| CN103204839B (en) | Synchronous preparation method of effective ingredient of licorice | |
| CN102633895B (en) | Extraction and preparation method by comprehensively utilizing liquorice | |
| CN103694364A (en) | Method for synchronously extracting, separating and purifying polysaccharides and flavones of cyclocarya paliurus | |
| CN102895303A (en) | Resin purification method for extracting and separating total flavone of cyclocarya paliurus | |
| CN104906165A (en) | Method for extracting platycodin | |
| CN101538296A (en) | Active ingredients of camptosorus sibiricus, and extraction method and use of same | |
| CN101792479B (en) | Process for extracting blood sugar reducing active saponin from cyclocarya paliurus | |
| CN104940280A (en) | Method for extracting total flavones from radix puerariae employing enzyme preparation | |
| CN102617696B (en) | Preparation method of asiaticoside | |
| CN103232515A (en) | Cyclocarya paliurus glucoside I preparation method | |
| CN101260133B (en) | Method for preparing hyperoside and isoquercetin from cotton petal | |
| CN108743657A (en) | The preparation method of methods of glycosides in a kind of mussot swertia herb | |
| CN101703554A (en) | Preparation and use of semen cuscutae flavonoids | |
| CN103989748A (en) | Method for extracting lotus seedpod procyanidins from lotus seedpod through full-low-temperature process | |
| CN102633860A (en) | Method for extracting ardisiacrispin A | |
| CN102718811A (en) | Preparation method of stilbene glycoside in polygonum cuspidatum | |
| CN102391330A (en) | Method for extracting liquiritin from liquorice | |
| CN102391232B (en) | The method of Liquiritigenin is extracted from Radix Glycyrrhizae | |
| CN104119410B (en) | A kind of processing method preparing aucubin monomer from bark of eucommia fruit | |
| CN102603826A (en) | Method for extracting 8-acetylharpagide from decumbent bugle herb plant | |
| CN102344474A (en) | Preparation method of paederia scandens glucoside | |
| CN102653537A (en) | Method for extracting and preparing high-purity silibinin from polygonum capitatum herb | |
| CN102010457A (en) | Method for preparing raddeanin A |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130130 |