CN1907935A - Purifying method of crude rhein - Google Patents
Purifying method of crude rhein Download PDFInfo
- Publication number
- CN1907935A CN1907935A CN 200610041105 CN200610041105A CN1907935A CN 1907935 A CN1907935 A CN 1907935A CN 200610041105 CN200610041105 CN 200610041105 CN 200610041105 A CN200610041105 A CN 200610041105A CN 1907935 A CN1907935 A CN 1907935A
- Authority
- CN
- China
- Prior art keywords
- solution
- rhein
- purification
- crude
- hour
- 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.)
- Granted
Links
Landscapes
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
Abstract
This invention involves a purification method for crude rhein, including a) adding alkali solution in the crude rhein at room temperature to obtain solution I, b) heating the solution I above to 63~66DEG C for 0.5-1 hours, c) adding excessive inorganic acid, heating to 83~95DEG C for 0.5-1 hours, and cooling to room temperature to obtain solution II, and d) filtering the solution II to obtain a filter cake, rinsing the filter cake by water repeatedly and drying at 90~95DEG C for 1-3 hours, and smashing to obtain the purified rhein. The invention has the advantages of simple operation, short production cycle, and low energy consumption, and is suitable for industrialized purification of rhein with low level (75-90%).
Description
Technical field
The present invention relates to a kind of method that improves crude rhein purity.Belong to technical field of medicament.
Background technology
Rhubarb yellow is the monomer of anthraquinone derivative, have functions such as antibiotic, antitumor, catharsis, diuresis, detoxifcation, anti-ageing, trapping Coxsackie B virus 3, immune two-ways regulation, arteriosclerosis, be considered to have the medicine of many target spots function, diabetes, ephrosis, obesity, hyperlipidemia, hypertension are had certain curative effect.Rhubarb yellow also is used to beauty culture as healthcare products, obtains abroad at present widely applying.Its---diacetyl rhein (diacerein), antitumor good medicine---main raw material of daunomycin, Zorubicin of still treating the good medicine of osteoarthropathy simultaneously.Rhubarb yellow generally all extracts from natural rheum officinale and obtains, to this existing patent report (CN1059893C, CN1282728A).Jiangyin Antarctic Star Biology Products Co., Ltd has begun to produce rhubarb yellow by synthetic route.No matter extraction method or synthesis method generally all adopt recrystallization method to the purification step of product.Recrystallization method exist solvent loss big, to defectives such as quality control less stable, the output of product are on the low side.Jiangyin Antarctic Star Biology Products Co., Ltd discloses a kind of process for purification (number of patent application: 200610039291.0) of rhubarb yellow, after rhubarb yellow being synthesized the bigger salt of solubleness, with inorganic acid reductive method rhubarb yellow is made with extra care again, remedied above-mentioned defective.Yet this process for purification exists the defective that reactions steps is many, the production cycle is long, energy consumption is high, only is applicable to the final refining of the crude product of rhubarb yellow content higher (more than 90%).
Summary of the invention
The objective of the invention is to overcome above-mentioned deficiency, provide a kind of easy and simple to handle, with short production cycle, energy consumption is low, be applicable to that the industrialization of rhubarb yellow content lower (75～90%) improves the method for crude rhein purity.
The object of the present invention is achieved like this: a kind of method of purification of crude rhein is characterized in that this method comprises following processing step:
A) in the rhubarb yellow crude product adding strong base solution, at room temperature form solution I,
B) above-mentioned solution I is warming up to 63～66 ℃, is incubated 0.5～1 hour,
C) insulation finishes the back and adds excessive inorganic strong acid solution, is incubated 0.5～1 hour after being warming up to 83～95 ℃, is cooled to room temperature again, forms solution II,
D) with above-mentioned solution II strainer suction filtration, the repeatedly laggard baking oven of filter cake water flushing, 90～95 ℃ of dryings 1～3 hour, the rhubarb yellow after promptly obtaining after the pulverizing purifying.
Highly basic of the present invention is potassium hydroxide or sodium hydroxide,
Inorganic acid of the present invention is sulfuric acid, hydrochloric acid or nitric acid, and is best with the hydrochloric acid effect.
Above-mentioned steps b) can decolorization filtering then effect is better if finish the back, but yield can decrease.
The present invention is by the rhubarb yellow crude product is dissolved in strong base solution, again with the inorganic acid reduction, thereby has realized improving the purpose of rhubarb yellow content in crude product, generally can improve content 5～18%.Content is most economical 75～90%.This method has characteristics such as easy and simple to handle, with short production cycle, that energy consumption is low, is highly suitable for industrialized production.
Embodiment
Embodiment 1:
A) 30 gram rhubarb yellow crude products (HPLC content 81%) are dropped into the 1000mL flask, add the potassium hydroxide solution that 30 gram potassium hydroxide are dissolved in 250mL water, stir, at room temperature form solution I,
B) above-mentioned solution I is warming up to 63～66 ℃, and is incubated 0.5 hour,
C) insulation finish to add the hydrochloric acid soln 200mL of 6N, stirs 3～4 minutes, adds entry 200mL again, is warming up to backflow (83～86 ℃) and keeps 0.5 hour, is cooled to room temperature (22～26 ℃) again, the formation solution II,
D) with above-mentioned solution II B suction filtration, filter cake is pulverized rhubarb yellow (HPLC content 92%) 25.6 grams after promptly obtaining purifying with 200mL water flushing three laggard baking ovens (≤95 ℃) drying after dry 2 hours.
Embodiment 2:
A) 60 gram rhubarb yellow crude products (HPLC content 79%) are dropped into the 2000mL flasks, add 45 gram sodium hydroxide be dissolved in 500mL water sodium hydroxide solution, stir, at room temperature form solution I,
B) above-mentioned solution I is warming up to 63～66 ℃, and is incubated 0.5 hour,
C) insulation finish to add the sulphuric acid soln 400mL of 3N, stirs 3～4 minutes, adds entry 400mL again, is warming up to 92～95 ℃ and kept 0.5 hour, is cooled to room temperature (22～26 ℃) again, the formation solution II,
D) with above-mentioned solution II B suction filtration, filter cake is pulverized rhubarb yellow (HPLC content 88%) 51.8 grams after promptly obtaining purifying with 200mL water flushing three laggard baking ovens (≤95 ℃) drying after dry 1 hour.
Embodiment 3:
A) 60 gram rhubarb yellow crude products (HPLC content 78%) are dropped into the 2000mL flasks, add 45 gram sodium hydroxide be dissolved in 500mL water sodium hydroxide solution, stir, at room temperature form solution I,
B) above-mentioned solution I is warming up to 63～66 ℃, and is incubated 1 hour, decolorization filtering while hot,
C) decolorization filtering finish to add the salpeter solution 400mL of 6N, stirs 3～4 minutes, adds entry 400mL again, is warming up to 90～92 ℃ and kept 1 hour, is cooled to room temperature (22～26 ℃) again, the formation solution II,
D) with above-mentioned solution II B suction filtration, filter cake is pulverized rhubarb yellow (HPLC content 89%) 51.7 grams after promptly obtaining purifying with 200mL water flushing three laggard baking ovens (≤95 ℃) drying after dry 3 hours.
Claims (5)
1, a kind of method of purification of crude rhein is characterized in that this method comprises following processing step:
A) in the rhubarb yellow crude product adding strong base solution, at room temperature form solution I,
B) above-mentioned solution I is warming up to 63～66 ℃, is incubated 0.5～1 hour,
C) insulation finishes the back and adds excessive inorganic strong acid solution, is incubated 0.5～1 hour after being warming up to 83～95 ℃, is cooled to room temperature again, forms solution II,
D) with above-mentioned solution II strainer suction filtration, the repeatedly laggard baking oven of filter cake water flushing, 90～95 ℃ of dryings 1～3 hour, the rhubarb yellow after promptly obtaining after the pulverizing purifying.
2, the method for purification of a kind of crude rhein according to claim 1 is characterized in that: the described highly basic of step a) is potassium hydroxide or sodium hydroxide.
3, the method for purification of a kind of crude rhein according to claim 1 and 2 is characterized in that: the described inorganic acid of step c) is sulfuric acid, hydrochloric acid or nitric acid.
4, the method for purification of a kind of crude rhein according to claim 1 and 2 is characterized in that: the step b) insulation finishes rear decoloring and filters.
5, the method for purification of a kind of crude rhein according to claim 1 and 2 is characterized in that: the described intensification temperature of step c) is 92～95 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100411057A CN100351220C (en) | 2006-08-03 | 2006-08-03 | Purifying method of crude rhein |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100411057A CN100351220C (en) | 2006-08-03 | 2006-08-03 | Purifying method of crude rhein |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1907935A true CN1907935A (en) | 2007-02-07 |
| CN100351220C CN100351220C (en) | 2007-11-28 |
Family
ID=37699191
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100411057A Expired - Fee Related CN100351220C (en) | 2006-08-03 | 2006-08-03 | Purifying method of crude rhein |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100351220C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106344549A (en) * | 2016-11-02 | 2017-01-25 | 江苏康缘药业股份有限公司 | Application of rhein in preparation of drugs for preventing and/or treating hand-foot-and-mouth disease |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1059893C (en) * | 1997-07-17 | 2000-12-27 | 中国人民解放军南京军区南京总医院 | Rheic acid extracting method from rhubarb and its purification process |
| CN1282728A (en) * | 1999-08-03 | 2001-02-07 | 兰州大学 | Process for extracting chrysophanic acid |
-
2006
- 2006-08-03 CN CNB2006100411057A patent/CN100351220C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106344549A (en) * | 2016-11-02 | 2017-01-25 | 江苏康缘药业股份有限公司 | Application of rhein in preparation of drugs for preventing and/or treating hand-foot-and-mouth disease |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100351220C (en) | 2007-11-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1900126A (en) | Process for preparing chitin and chitosan | |
| CN1715255A (en) | Method for producing chitin, astaxanthin, protein, calcium powder and biological fertilizer from shrimp shell | |
| CN1896262A (en) | Technology of animal high-calcium powder, chondrine and collagen by composite enzyme method | |
| CN1830996A (en) | Method for preparing chenodeoxycholic acid | |
| CN101037485A (en) | Pectin extraction method | |
| CN1896255A (en) | Extraction of high-purity resveratrol by converting microbion into polydatin material | |
| CN1827755A (en) | Preparation method of scallop splanchna active components | |
| CN100351220C (en) | Purifying method of crude rhein | |
| CN1869043A (en) | Synthesis method of chenodeoxycholic acid | |
| CN115197287A (en) | Method for comprehensively extracting rubusoside, quercetin and ellagic acid from sweet tea and application thereof | |
| CN107382937B (en) | Method for extracting luteolin from luteolin | |
| CN1261413C (en) | Purification process for 5-[pair-(2-pyridine sulfamic) benzene] azo salicylic acid | |
| CN1156465C (en) | Extraction technology of new stellerin A | |
| CN115975066B (en) | Production method and application of food-grade tremella polysaccharide | |
| CN100345856C (en) | Esterification and crystallizing process for producing glucose halfaldehyde lactone | |
| CN117210971A (en) | Method for preparing high-water-holding capacity and high-oil-holding capacity nano citrus fiber | |
| CN100351222C (en) | Rheinic acid preparing process | |
| CN102432575A (en) | Method for extracting high-purity hesperetin from immature bitter orange | |
| CN105541951A (en) | Method for refining obeticholic acid | |
| CN113061196B (en) | Method for extracting sodium alginate by high-pressure homogenization | |
| CN1493571A (en) | Luteolin metal salt and its preparation method and use | |
| CN104432109A (en) | Method for preparing sulfated water-soluble dietary fiber employing extrusion | |
| CN1253462C (en) | Process for preparing morinda officinalis total oligosaccharide | |
| CN103483404A (en) | Method for extracting and purifying hesperidin from orange residues | |
| CN101041842A (en) | Clean production method of chondroitin sulfate and protein |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20071128 Termination date: 20150803 |
|
| EXPY | Termination of patent right or utility model |