CN1059893C - Rheic acid extracting method from rhubarb and its purification process - Google Patents
Rheic acid extracting method from rhubarb and its purification process Download PDFInfo
- Publication number
- CN1059893C CN1059893C CN97107047A CN97107047A CN1059893C CN 1059893 C CN1059893 C CN 1059893C CN 97107047 A CN97107047 A CN 97107047A CN 97107047 A CN97107047 A CN 97107047A CN 1059893 C CN1059893 C CN 1059893C
- Authority
- CN
- China
- Prior art keywords
- extracting
- rhubarb
- yellow
- hydrochloric acid
- ether
- 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.)
- Expired - Fee Related
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention discloses a method for extracting and purifying rhein as an effective component from rhubarb as a Chinese medicine. The method comprises the steps: roots and stems of rhubarb are sliced; diluted alcohol is used for extraction, and the alcohol is evaporated out; concentrated liquid is hydrolyzed with hydrochloric acid; ether is used for extracting hydrolyzing liquid; diluted bicarbonate solution is used for extracting rhein from the ether; bicarbonate extracting liquid is acidified; crude rhein is precipitated out; after the recrystallization is carried out in acetic acid, yellow needle crystals are obtained, and the melting point is from 318 to 320 DEG C.
Description
The present invention relates to anthraquinone derivative, is a kind of carboxylic acid of anthraquinone, specifically, is to extract from Chinese herb rhubarb and the method for purifying rhubarb yellow.
Ancient Chinese generation just with Radix Et Rhizoma Rhei or process of preparing Chinese medicine rheum officinale be used as medicine (see " Chinese patent medicine research " 1983, NO.5,11-12).
In recent years reported the research (" bulletin of Chinese materia medica " VOL.12 (5), 286-288,1987) of from rheum officinale, extracting Radix Et Rhizoma Rhei anthraquinone.Shang Weiyou extracts, isolates the report of rhubarb yellow from rheum officinale.
Commercially available rheum officinale Chinese patent medicine is the hybrid medicine that extracts from rheum officinale.Though these preparations are effective, curative effect instability, and the component of failing to remove toxic side effect.
The purpose of this invention is to provide a kind of from rheum officinale extraction separation go out single effective ingredient rhubarb yellow
Rhein) method.
Technical scheme of the present invention is as follows:
A kind of extracting and purifying method of rhubarb yellow, it is with the root of rheum officinale, stem section, add alcoholic extraction, can be with the ethanol aqueous solution more than 40%, extraction can be carried out at 10-80 ℃, extracting solution boils off alcohol, be condensed into rare syrupy shape, add concentrated hydrochloric acid hydrolysis, hydrolysis can be carried out at 40-70 ℃, and hydrolysis can be finished the hydrolyzed solution ether extraction at 0.5-2.0 hour, extract rhubarb yellow in the ether extracted liquid with rare bicarbonate solution again, be acidified with acid the rough rhubarb yellow that the supercarbonate extracting solution obtains yellow mercury oxide.Rough rhubarb yellow washes with water, gets the reddish-brown powder after the drying, wherein contains rhubarb yellow and is about 50%.
Rough rhubarb yellow gets yellow needle-like crystal after using the acetic acid recrystallization, and fusing point is 318-320 ℃.
Adopt the extracting and purifying method of rhubarb yellow of the present invention, can be easily extract from rheum officinale, purifying obtains rhubarb yellow, as medicine, it is evident in efficacy, and has reduced the toxic side effect of rheum officinale.
Embodiment:
Select Gansu to produce 1 kilogram on sorrel root, stem, be cut into the 2-5mm thin slice after water is moistening, put in the extractor, add 50% ethanol 2000ml, reflux 6 hours is transferred to extracting solution in the decompression still, steams alcohol, steams to 1/3 of original volume, is rare syrupy shape.Under agitation add concentrated hydrochloric acid (11.7mol/L), the rheum officinale concentrated solution of 20 parts of volumes adds the concentrated hydrochloric acid of 1 volume, and 50 ℃ of hydrolysis 1 hour, cooling back was with isopyknic ether extraction 2 times, and the merging ether extracted liquid is used and the isopyknic 5%NaHCO of ether
3Extract 1 time, at NaHCO
3Add concentrated hydrochloric acid (11.7mol/L) to PH2 under stirring in the extracting solution, obtain yellow mercury oxide, leave standstill more than 4 hours, the supernatant liquid that inclines, suction filtration goes out precipitation, washes with water to washings to be neutral, get pulverous thick yellow acid 10 grams of reddish-brown after the drying, content is about 50%.(1: 1v/v) mixed solution washs thick yellow acid (the thick yellow acid of per 100 grams 5ml alcohol one ketone mixed solution), uses the acetic acid recrystallization behind the suction filtration, gets yellow needle-like crystal 5 grams, and fusing point is with ethanol one acetone; 318-320 ℃, stratographic analysis shows consistent with the rhubarb yellow standard substance.
Claims (3)
1. the extracting and purifying method of a rhubarb yellow, it is characterized in that root, stem section with rheum officinale, the ethanol aqueous solution that adds more than 40% extracts, extracting solution boils off alcohol, add concentrated hydrochloric acid hydrolysis, the hydrolyzed solution ether extraction extracts rhubarb yellow in the ether extracted liquid with rare bicarbonate solution again, be acidified with acid the supercarbonate extracting solution, obtain the rough rhubarb yellow of yellow mercury oxide.
2. extracting and purifying method according to claim 1 is characterized in that adding alcoholic extraction and carries out at 10-80 ℃.
3. extracting and purifying method according to claim 1, it is characterized in that adding concentrated hydrochloric acid hydrolysis is the concentrated hydrochloric acid that adds 11.7MOL/L, 40-70 ℃ hydrolysis 0.5-2.0 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97107047A CN1059893C (en) | 1997-07-17 | 1997-07-17 | Rheic acid extracting method from rhubarb and its purification process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97107047A CN1059893C (en) | 1997-07-17 | 1997-07-17 | Rheic acid extracting method from rhubarb and its purification process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1205999A CN1205999A (en) | 1999-01-27 |
| CN1059893C true CN1059893C (en) | 2000-12-27 |
Family
ID=5169237
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97107047A Expired - Fee Related CN1059893C (en) | 1997-07-17 | 1997-07-17 | Rheic acid extracting method from rhubarb and its purification process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1059893C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100351220C (en) * | 2006-08-03 | 2007-11-28 | 江阴南极星生物制品有限公司 | Purifying method of crude rhein |
| CN102924270A (en) * | 2012-03-18 | 2013-02-13 | 兰州大学 | Method for extracting rhein from rheum |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100450990C (en) * | 2006-03-31 | 2009-01-14 | 江阴南极星生物制品有限公司 | Method for treating asphalt like slag in preparing rheinic acid and diacerein process with aloe |
| CN101898961A (en) * | 2009-05-31 | 2010-12-01 | 中国医学科学院药物研究所 | Parietic acid crystal C type solid matter as well as preparation method and application thereof |
| CN102188501B (en) * | 2011-04-29 | 2013-01-02 | 栗进才 | Rhubarb anthraquinones component extracting and separating method |
-
1997
- 1997-07-17 CN CN97107047A patent/CN1059893C/en not_active Expired - Fee Related
Non-Patent Citations (5)
| Title |
|---|
| 《中成药研究》1989年第5期 1983.1.1 黄泰康，中药大黄炮制沿革的研究 * |
| 《中药通报》第12卷第5期 1987.5.1 罗顺德等，几种提取方法对大黄葸醌含量的影响 * |
| 《大黄提取工艺的研究》傅莲瑛等 * |
| 《天津药学》1996年第8卷第4期 1996.1.1 * |
| 《天津药学》1996年第8卷第4期 1996.1.1;《大黄提取工艺的研究》傅莲瑛等;《中成药研究》1989年第5期 1983.1.1 黄泰康，中药大黄炮制沿革的研究;《中药通报》第12卷第5期 1987.5.1 罗顺德等，几种提取方法对大黄葸醌含量的影响 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100351220C (en) * | 2006-08-03 | 2007-11-28 | 江阴南极星生物制品有限公司 | Purifying method of crude rhein |
| CN102924270A (en) * | 2012-03-18 | 2013-02-13 | 兰州大学 | Method for extracting rhein from rheum |
| CN102924270B (en) * | 2012-03-18 | 2014-09-03 | 兰州大学 | Method for extracting rhein from rheum |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1205999A (en) | 1999-01-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108341887B (en) | Preparation method of dendrobium huoshanense polysaccharide | |
| CN1813802A (en) | Bufonid skin extract production process | |
| CN101007797B (en) | Method for extracting dihydromyricetin from Japanese raisin tree seed | |
| CN1059893C (en) | Rheic acid extracting method from rhubarb and its purification process | |
| JP2022545288A (en) | Tea composition for prevention, improvement or effect of respiratory disease and pharmaceutical composition containing the same | |
| CN1313479C (en) | Method for preparing holothurin from waste solution of sea cucumber processing | |
| CN105504079A (en) | Process for producing astragalus polysaccharide by using ultrasonic technology | |
| CN1425643A (en) | Extracting and purifying method for chlorogenic acid in honeysuckle | |
| CN1359905A (en) | Process for extracting licoflavone, lycyrrhizic acid and licopolyose from liquorice root | |
| CN108517018A (en) | A kind of PERICARPIUM TRICHOSANTHIS active constituent extraction process | |
| JP2016026203A (en) | Picrorhiza kurroa extract for prevention, elimination and treatment of rna viruses and infections or diseases caused by the same, in humans, animals, and biotechnology industry | |
| CN1102025C (en) | Formula of liver-protecting milk powder and its production process | |
| CN105399852A (en) | Technology for producing radix astragali polysaccharide by utilization of alkaline process extraction technology | |
| CN105175243A (en) | Method for purifying pinolenic acid from pine seed oil | |
| CN110144017B (en) | Continuous preparation process of active ingredients in bamboo fungus spores | |
| CN107982310A (en) | The preparation method of compound kudzu root flavones preparation | |
| CN106943466A (en) | A kind of extracting method of active ingredients from traditional Chinese medicinal | |
| CN1235852C (en) | Method for extracting curcumin from peltate yam | |
| CN105440148A (en) | Process for producing astragalus polysaccharide by using water extraction technology | |
| CN104173510A (en) | Preparation method of jute-semen armeniacae amarae-gypsum-liquorice oral solution | |
| CN103214538B (en) | The separation purification method of mating type total cholic acid in a kind of courage cream | |
| CN1237973C (en) | Chronic bronchitis treating traditional Chinese medicine | |
| CN1552722A (en) | Method for extracting and separating oleanolic acid | |
| CN102532083A (en) | Preparation process for formononetin with high purity | |
| CN1660832B (en) | Method for extracting and separating general flavone and saponin astragalus root from astragalus root |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |