CN1772752A - Clean kurarinol producing process - Google Patents
Clean kurarinol producing process Download PDFInfo
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- CN1772752A CN1772752A CN 200510113090 CN200510113090A CN1772752A CN 1772752 A CN1772752 A CN 1772752A CN 200510113090 CN200510113090 CN 200510113090 CN 200510113090 A CN200510113090 A CN 200510113090A CN 1772752 A CN1772752 A CN 1772752A
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- Prior art keywords
- matrine
- kurarinol
- oxidation
- clean
- liquid
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Abstract
The clean kurarinol producing process with matrine as material includes the technological steps of: oxidation, quenching, extracting to recover matrine, concentrating, re-dissolving in polar solvent, filtering, concentration to crystallize, separation and stoving and refining. The step of extracting to recover matrine is to extract residual matrine in the oxidation reacted liquid with non-polar organic solvent before returning the extracted liquid to the oxidation step. The separated mother liquid after concentration to crystallize is returned to the matrine refining section. The quenching step has catalyst for terminating reaction to the oxidation reacted liquid and the catalyst is reducing compound. Compared with available technology, the present invention has the advantages of simple technological process, short production period, high product yield, raised production efficiency and no waste liquid exhaust.
Description
Technical field: the invention belongs to the Chinese herbal medicine extracting processing technique field, particularly use the method for the matrine production kurarinone that from Herba Sophorae alopecuroidis, extracts, a kind of clean kurarinol producing process.
Background technology: kurarinone is a kind of alkaloid that extracts preparation from the Chinese medicine Herba Sophorae alopecuroidis, and wherein Oxymatyine (oxymatrine) accounts for more than 98%, and molecular formula is C
15H
24N
2O
2.H
2O, molecular weight are 282, and other also have the sophocarpine of minute quantity.Clinical study shows: kurarinone has direct anti-hepatitis B virus effect, has the collagen mobility of inhibition and fibrosis effect in the time of Oxymatyine treatment chronic hepatitis.Oxymatyine also has antianaphylaxis, anti-inflammatory action: can regulate immunity and leukocyte increasing; In December, 1996 is by the specified attached Huashan hospital of medical university of going up of the Ministry of Health, Beijing You An hospital finishes 40 routine randomized, double-blind checking and other basic demonstrations about drug effect, untoward reaction, and Ministry of Health's approval on February 24th, 1998 Oxymatyine is country's treatment chronic hepatitis B five kind new medicines; In August, 1998 China medical association emphasis popularization engineering specialist authenticates decision and lists the Treated by Oxymatrine Injection viral hepatitis in emphasis popularization engineering project, promotes the use of in the whole nation;
At present kurarinone how adopts with the matrine that to be raw material synthesize through processing steps such as oxidation, extraction, concentrated, backflow, suction filtrations; In all disclosed patent documentations, all used excessive hydrogen peroxide oxidant, as number of patent application 96109730.2 and 00109240.5 patent of invention bulletin; Facts have proved: excessive hydrogen peroxide is not as removing, can make in the product kurarinone remaining content of hydrogen peroxide too high, has toxicity, can not use as bulk drug, and alkaline matter decomposition of hydrogen peroxide such as use sodium hydroxide, when temperature is hanged down, reaction times is longer, by product was a lot of when temperature was high, caused the aftertreatment difficulty, and product yield reduces.
Summary of the invention: the objective of the invention is to overcome the prior art defective provides a kind of technology simple, easy and simple to handle, and production cost is lower, productive rate height, the clean kurarinol producing process that no discharging of waste liquid is circulating.
Purpose of the present invention realizes by following scheme:
Clean kurarinol producing process, with the matrine is raw material, technological process is: oxidation, cancellation, extraction are reclaimed matrine, are concentrated, heavy molten, the filtration of polar solvent, condensing crystal, separation oven dry, crude product refining, it is that extraction liquid returns oxidation section with remaining matrine in the non-polar organic solvent extraction oxidation liquid that the matrine process is reclaimed in extraction; The isolated mother liquor of condensing crystal returns the refining workshop section of matrine;
Above-mentioned cancellation process is the catalyzer that adds termination reaction in oxidation liquid, and this catalyzer is a reducing compound;
The used oxygenant of above-mentioned oxidising process is a hydrogen peroxide, and the weight proportion of matrine and the reaction of industrial hydrogen peroxide is: 1: 0.8-1.0;
Above-mentioned non-polar organic solvent is ether, sherwood oil or benzene kind solvent;
Above-mentioned reducing compound is sodium sulphite, Sulfothiorine, S-WAT or sodium iodide, and addition is the 0.5-2% of the used weight of matrine.
Above-mentioned polar organic solvent is an alcoholic solvent.
The present invention compared with prior art, technology is simpler, the production cycle is shorter, be 1/3 of primitive period, product yield height, prior art products yield about 50%, the present invention can reach more than 80%, and corresponding production efficiency improves a lot, and production whole process does not in addition have discharging of waste liquid.
Embodiment:
Embodiment 1:
Matrine 10kg slowly joins 10kg technical grade (content about 30%) H
2O
2In the solution, in 50-80 ℃ stir 48 hours after, add cancellation catalyst vulcanization sodium 0.05kg and finish reaction, with 500kg extracted with diethyl ether oxidation liquid no matrine colour developing spot to the oxidation liquid, the heating of oxidation liquid is concentrated into dried, add 10-20kg ethanol to kurarinone and dissolve fully, after filtering insolubles, concentrate dissolve with ethanol liquid, add and help crystallizing agent 20-25kg ethyl acetate to help its crystallization, promptly get the kurarinone product after centrifugal.After mother liquor concentrates, carry out secondary crystal, reclaim product, after filtration, product is heavy molten with acetone, the product that recrystallization can obtain to be up to state standards.Collect all remaining mother liquors and return matrine purifying workshop section.
Embodiment 2:
In reactor, add 8kg H
2O
2Solution slowly adds matrine 10kg under stirring; The controlled oxidation temperature stirs after 40-90 hour for 30-80 ℃, and the cancellation catalyzer is selected 0.1kg Sulfothiorine for use, helps crystallizing agent to select acetone for use, and other technology is identical with example 1.
Embodiment 3:
In reactor, add 8kg H
2O
2Solution slowly adds matrine 10kg under stirring; 40-90 ℃ of controlled oxidation temperature stirred after 40-90 hour, and the cancellation catalyzer is selected the 0.2kg S-WAT for use, and with 500kg petroleum ether extraction oxidation liquid no matrine to the oxidation liquid spot that develops the color, other technology is identical with example 1.
Embodiment 4:
In reactor, add 9kg H
2O
2Solution slowly adds matrine 10kg under stirring; 40-90 ℃ of controlled oxidation temperature stirred after 40-90 hour, and the cancellation catalyzer is selected the 0.15kg sodium iodide for use, and with 500kg toluene extraction oxidation liquid no matrine to the oxidation liquid spot that develops the color, other technology is identical with example 1.
Claims (5)
1, clean kurarinol producing process, with the matrine is raw material, technological process is: oxidation, cancellation, extraction are reclaimed matrine, are concentrated, heavy molten, the filtration of polar solvent, condensing crystal, separation oven dry, crude product refining, it is characterized in that extracting recovery matrine process is that extraction liquid returns oxidation section with remaining matrine in the non-polar organic solvent extraction oxidation liquid; The isolated mother liquor of condensing crystal returns the refining workshop section of matrine; Above-mentioned cancellation process is the catalyzer that adds termination reaction in oxidation liquid, and this catalyzer is a reducing compound.
2, clean kurarinol producing process as claimed in claim 1 is characterized in that the used oxygenant of above-mentioned oxidising process is a hydrogen peroxide, and the weight proportion of matrine and the reaction of industrial hydrogen peroxide is: 1: 0.8-1.0.
3, clean kurarinol producing process as claimed in claim 1 is characterized in that above-mentioned non-polar organic solvent is ether or benzene kind solvent.
4, clean kurarinol producing process as claimed in claim 1 is characterized in that above-mentioned reducing compound is sodium sulphite, Sulfothiorine, S-WAT or sodium iodide, and addition is the 0.5-2% of the used weight of matrine.
5, clean kurarinol producing process as claimed in claim 1 is characterized in that above-mentioned polar organic solvent is an alcoholic solvent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101130906A CN100402527C (en) | 2005-10-13 | 2005-10-13 | Clean kurarinol producing process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101130906A CN100402527C (en) | 2005-10-13 | 2005-10-13 | Clean kurarinol producing process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1772752A true CN1772752A (en) | 2006-05-17 |
| CN100402527C CN100402527C (en) | 2008-07-16 |
Family
ID=36759911
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005101130906A Expired - Fee Related CN100402527C (en) | 2005-10-13 | 2005-10-13 | Clean kurarinol producing process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100402527C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102285987A (en) * | 2011-08-15 | 2011-12-21 | 江苏天晟药业有限公司 | Novel preparation process of oxymatrine |
| CN114591329A (en) * | 2022-03-03 | 2022-06-07 | 北京岳达生物科技有限公司 | Mutual transformation method of sophora flavescens effective components |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1277202A (en) * | 2000-06-19 | 2000-12-20 | 宁夏药物研究所 | Matrinidine and its preparation technology |
-
2005
- 2005-10-13 CN CNB2005101130906A patent/CN100402527C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102285987A (en) * | 2011-08-15 | 2011-12-21 | 江苏天晟药业有限公司 | Novel preparation process of oxymatrine |
| CN114591329A (en) * | 2022-03-03 | 2022-06-07 | 北京岳达生物科技有限公司 | Mutual transformation method of sophora flavescens effective components |
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| Publication number | Publication date |
|---|---|
| CN100402527C (en) | 2008-07-16 |
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| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20080716 Termination date: 20111013 |