CN102617575A - Preparation process of high-purity oxymatrine - Google Patents
Preparation process of high-purity oxymatrine Download PDFInfo
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- CN102617575A CN102617575A CN2012101011127A CN201210101112A CN102617575A CN 102617575 A CN102617575 A CN 102617575A CN 2012101011127 A CN2012101011127 A CN 2012101011127A CN 201210101112 A CN201210101112 A CN 201210101112A CN 102617575 A CN102617575 A CN 102617575A
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- matrine
- oxymatyine
- oxide
- preparation technology
- high purity
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Abstract
The invention provides a preparation process of high-purity oxymatrine. The method comprises the following steps of: firstly, heating purified water in a water bath to a certain temperature; adding hydrogen peroxide and slowly adding oxymatrine to react at the certain temperature until the hydrogen peroxide is completely consumed; then, extracting residual less oxymatrine; decompressing and concentrating a reaction solution and adding an alcohols substance into the concentrated solution to be dissolved; adding a de-coloring agent for decoloring and filtering; continually decompressing and concentrating; adding an acetones substance to crystallize; and re-crystallizing to obtain the oxymatrine. The process method disclosed by the invention has the advantages of simplicity and practical applicability, low cost and high yield; and more importantly, the purity is high and the preparation process is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of preparation technology of high purity matrine oxide.
Background technology
Chinese medicine kuh-seng, Herba Sophorae alopecuroidis, Sophora Alopecuroides L. belong to leguminous plants, and the three has heat-clearing and damp-drying drug as the main source of Oxymatyine, the effect of desinsection, diuresis.Wherein mainly contain vegeto-alkali and flavones ingredient in the kuh-seng.Pharmacological evaluation proof total alkaloids has arrhythmia and antitumour activity etc.Contain a large amount of matrines in the kuh-seng, what wherein content was the highest is matrine and Oxymatyine, also has other close vegeto-alkali simultaneously, and it mainly is other biological alkali compositions such as sophocarpine, sophoramine, sophorine, Iosmatrine.
Oxymatyine has another name called kurarinone, molecular formula C
15H
24N
2O
2, prismatic crystal of white needles or white crystalline powder, odorless, bitter.One of vegeto-alkali that this strain is separated from pulse family platymiscium kuh-seng, Herba Sophorae alopecuroidis, Sophora Alopecuroides L..Can be used for treating the white corpuscle that causes because of tumor radiotherapy, chemotherapy and lowly reach the leukopenia that other reasons cause; Be used for treatment and the eczema of chronic viral hepatitis B, the treatment of contact dermatitis.
Oxymatyine has very high pharmaceutical use, and its its preparation process is reported in patent documentation and be few, and the Oxymatyine purity of preparation can only reach 98%; CN1111533C for example; Open day is on June 18th, 2003, points out the Oxymatyine for preparing in the reality, and its purity can not reach more than 99%; Thereby do not possess practicality, and point out reaching more than 99% when none kind preparation technology of fashion can make purity.
Summary of the invention
The objective of the invention is in order to overthrow the technological judgement among the CN1111533C, and overcome the defective of prior art, a kind of preparation technology of high purity matrine oxide is provided, its purity can reach more than 99.5%.
For realizing above-mentioned purpose, the present invention takes following technical scheme:
For matrine is fully reacted; Reach the yield supreme good; Earlier in oxidation tank, add the water heating in water bath, be metered into ydrogen peroxide 50, and slowly add water crystallization matrine bullion and dissolve; Because of water crystallization matrine bullion need add the matrine elaboration than other preparation Oxymatyines, reduce production costs greatly.Cool to certain temperature then, isothermal reaction till do not have a ydrogen peroxide 50, extraction residue matrine; Vacuum decompression concentration of reaction solution, liquid concentrator add the alcohols material dissolving, and for making these article color purer, quality is higher, and lysate need pass through the glass tower decolouring that contains discoloring agent, suction filtration (in case the decolouring material is residual); Vacuum decompression concentrates once more, and the crystallization of adding recrystallisation solvent, recrystallization get high purity, high yield, high-quality Oxymatyine.
A kind of preparation technology of high purity matrine oxide, concrete steps are:
(1) oxidation tank adds the water bath temperature and rises to 75 ℃, and metering adds ydrogen peroxide 50, slowly adds matrine and dissolves, and cools the temperature to 58-62 ℃ of isothermal reaction;
(2) oxidation liquid reaction extracts unreacted matrine with the benzene class after do not have ydrogen peroxide 50, in oxidation liquid, do not have matrine basically till;
(3) vacuum decompression concentration of reaction solution adds ethanol class substance dissolves, suction filtration;
(4) filtrating is through bleaching agent bleaching, suction filtration;
(5) vacuum decompression concentrates, and add recrystallisation solvent and stir, crystallisation by cooling, spinning gets the Oxymatyine bullion;
(6) the Oxymatyine bullion is added dissolve with ethanol, ethanol liquid is through bleaching agent bleaching, and suction filtration reclaims ethanol, and add recrystallisation solvent and stir, crystallisation by cooling, spinning gets the Oxymatyine elaboration.
Said ydrogen peroxide 50 is common ydrogen peroxide 50 or analytical pure ydrogen peroxide 50.
Said benzene class is toluene, benzene.
Said matrine is matrine elaboration or water crystallization matrine bullion.
Said discoloring agent is gac or aluminium oxide Al
2O
3
Said recrystallisation solvent is acetone, ethanol, methyl alcohol, ETHYLE ACETATE.
The present invention has the following advantages:
(1) product purity is high: calculate with dry product, gained Oxymatyine purity can reach more than 99.5%, has broken through traditional purity that can not reach of thinking.
(2) proterties is good: adopt bleaching agent bleaching, filter, product color is good, the crystal homogeneous.
(3) prescription is reasonable, practical: because it is higher to use the matrine elaboration to prepare Oxymatyine cost on suitability for industrialized production; So the present invention can directly utilize water crystallization matrine bullion to prepare high purity matrine oxide; Both scientific and reasonable, practical, can guarantee its quality again.
(4) preparation technology is simple, cost is low, quality is high, is applicable to suitability for industrialized production.
Description of drawings
Accompanying drawing 1 is process flow sheet of the present invention.
Embodiment
Embodiment 1:
Add water heating in water bath to 75 ℃ in the oxidation tank, add analytical pure ydrogen peroxide 50 51g, slowly add water crystallization matrine bullion 100g; After 13 hours,, in reaction solution, there is not matrine basically in 61 ℃ of reactions with the intact matrine of extracted in toluene unreacted; Vacuum decompression concentrates, and reclaims moisture to doing; Add dissolve with ethanol, add aluminium sesquioxide (Al
2O
3) the 30g decolouring, suction filtration; Vacuum decompression concentrates again, reclaims ethanol to doing, and adds acetone hot melt, crystallisation by cooling; Spinning gets Oxymatyine bullion 101g, and the Oxymatyine bullion is added dissolve with ethanol, and ethanol liquid is through bleaching agent bleaching; The suction filtration destainer reclaims ethanol, adds acetone and stirs; Crystallisation by cooling, spinning get Oxymatyine elaboration 95g, and assay is 99.9%.
Embodiment 2:
Add water heating in water bath to 75 ℃ in the oxidation tank, add analytical pure ydrogen peroxide 50 51g, slowly add water crystallization matrine bullion 100g; After 12 hours,, in reaction solution, there is not matrine basically in 59 ℃ of reactions with the intact matrine of benzene extraction unreacted; Vacuum decompression concentrates, and reclaims moisture to doing.Add dissolve with ethanol, add aluminium sesquioxide (Al
2O
3) the 30g decolouring, suction filtration; Vacuum decompression concentrates again, reclaims ethanol to doing, and adds acetone hot melt, crystallisation by cooling; Spinning gets Oxymatyine bullion 97g, and the Oxymatyine bullion is added dissolve with ethanol, and ethanol liquid is through bleaching agent bleaching; The suction filtration destainer reclaims ethanol, adds acetone and stirs; Crystallisation by cooling, spinning get Oxymatyine elaboration 92.8g, and assay is 99.7%.
Embodiment 3:
Add water heating in water bath to 75 ℃ in the oxidation tank, add analytical pure ydrogen peroxide 50 51g, slowly add water crystallization matrine bullion 100g; After 12 hours,, in reaction solution, there is not matrine basically in 62 ℃ of reactions with the intact matrine of extracted in toluene unreacted; Vacuum decompression concentrates, and reclaims moisture to doing.Add dissolve with ethanol, add aluminium sesquioxide (Al
2O
3) the 30g decolouring, suction filtration; Vacuum decompression concentrates again, reclaims ethanol to doing, and adds acetone hot melt, crystallisation by cooling, spinning and gets Oxymatyine bullion 101g; The Oxymatyine bullion is added dissolve with ethanol, and ethanol liquid is through bleaching agent bleaching, the suction filtration destainer; Reclaim ethanol, add acetone and stir crystallisation by cooling; Spinning gets Oxymatyine elaboration 95.6g, and assay is 100%.
Claims (5)
1. the preparation technology of a high purity matrine oxide, concrete steps are:
(1) oxidation tank adds the water bath temperature and rises to 75 ℃, is metered into ydrogen peroxide 50, slowly adds matrine then it is dissolved, and cools the temperature to 58-62 ℃ of isothermal reaction;
(2) oxidation liquid reaction is not after have ydrogen peroxide 50, with the matrine that benzene class extraction unreacted finishes, in oxidation liquid, do not have matrine basically till;
(3) vacuum decompression concentration of reaction solution adds the ethanol substance dissolves, suction filtration;
(4) filtrating is through bleaching agent bleaching, suction filtration;
(5) vacuum decompression concentrates, and adds recrystallisation solvent and stirs crystallisation by cooling, the Oxymatyine bullion of spinning;
(6) the Oxymatyine bullion is added alcohol solvent, ethanol liquid is through bleaching agent bleaching, and the suction filtration destainer reclaims ethanol, adds acetone and stirs crystallisation by cooling, the Oxymatyine elaboration of spinning.
2. the preparation technology of a kind of high purity matrine oxide as claimed in claim 1 is characterized in that the ydrogen peroxide 50 in said (1) step is common ydrogen peroxide 50, analytical pure ydrogen peroxide 50.
3. the preparation technology of a kind of high purity matrine oxide as claimed in claim 1 is characterized in that the benzene class is meant benzene, toluene in said (2) step.
4. the preparation technology of a kind of high purity matrine oxide as claimed in claim 1 is characterized in that the matrine in said (1) step is matrine elaboration, water crystallization matrine bullion.
5. the preparation technology of a kind of high purity matrine oxide as claimed in claim 1 is characterized in that the discoloring agent in said (4) step is gac, aluminum oxide (Al
2O
3).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101011127A CN102617575A (en) | 2012-04-10 | 2012-04-10 | Preparation process of high-purity oxymatrine |
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|---|---|---|---|
| CN2012101011127A CN102617575A (en) | 2012-04-10 | 2012-04-10 | Preparation process of high-purity oxymatrine |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102863443A (en) * | 2012-08-22 | 2013-01-09 | 宁夏紫荆花制药有限公司 | Method for preparing high-purity high-yield oxysophoridine |
| CN103113370A (en) * | 2013-02-28 | 2013-05-22 | 苏州农业职业技术学院 | Method for purifying baptifoline from radix sophorae flavescentis |
| CN103159767A (en) * | 2013-02-28 | 2013-06-19 | 苏州农业职业技术学院 | Method for extracting bap-iifoline from sophora flavescens |
| CN107376805A (en) * | 2017-08-14 | 2017-11-24 | 陕西昂煦生物科技有限公司 | A kind of matrine petroleum ether crystal system and its production technology |
| CN110256431A (en) * | 2019-07-16 | 2019-09-20 | 山东花物堂生物科技有限公司 | The extraction of biology total alkali and separation purifying technique in a kind of kuh-seng |
| 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 |
| CN115368353A (en) * | 2022-08-31 | 2022-11-22 | 陕西省西安植物园 | Separation and purification method of oxymatrine and oxysophocarpine mixture |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1310181A (en) * | 2000-11-18 | 2001-08-29 | 宁夏药物研究所 | Preparation of matrine oxide |
-
2012
- 2012-04-10 CN CN2012101011127A patent/CN102617575A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1310181A (en) * | 2000-11-18 | 2001-08-29 | 宁夏药物研究所 | Preparation of matrine oxide |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102863443A (en) * | 2012-08-22 | 2013-01-09 | 宁夏紫荆花制药有限公司 | Method for preparing high-purity high-yield oxysophoridine |
| CN103113370A (en) * | 2013-02-28 | 2013-05-22 | 苏州农业职业技术学院 | Method for purifying baptifoline from radix sophorae flavescentis |
| CN103159767A (en) * | 2013-02-28 | 2013-06-19 | 苏州农业职业技术学院 | Method for extracting bap-iifoline from sophora flavescens |
| CN103113370B (en) * | 2013-02-28 | 2015-03-25 | 苏州农业职业技术学院 | Method for purifying baptifoline from radix sophorae flavescentis |
| CN107376805A (en) * | 2017-08-14 | 2017-11-24 | 陕西昂煦生物科技有限公司 | A kind of matrine petroleum ether crystal system and its production technology |
| CN110256431A (en) * | 2019-07-16 | 2019-09-20 | 山东花物堂生物科技有限公司 | The extraction of biology total alkali and separation purifying technique in a kind of kuh-seng |
| 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 |
| CN115368353A (en) * | 2022-08-31 | 2022-11-22 | 陕西省西安植物园 | Separation and purification method of oxymatrine and oxysophocarpine mixture |
| CN115368353B (en) * | 2022-08-31 | 2024-04-12 | 陕西省西安植物园 | Separation and purification method of mixture of oxymatrine and sophocarpine |
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Application publication date: 20120801 |