CN102766143A - Method for extracting oxymatrine from Sophora moorcroftiana seeds - Google Patents
Method for extracting oxymatrine from Sophora moorcroftiana seeds Download PDFInfo
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- CN102766143A CN102766143A CN2012102703661A CN201210270366A CN102766143A CN 102766143 A CN102766143 A CN 102766143A CN 2012102703661 A CN2012102703661 A CN 2012102703661A CN 201210270366 A CN201210270366 A CN 201210270366A CN 102766143 A CN102766143 A CN 102766143A
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Abstract
The invention discloses a method for extracting oxymatrine from Sophora moorcroftiana seeds, comprising the steps of alkalifying, extracting, dissolving, crystallizing and post-treatment, wherein the specific steps are as follows: alkalifying Sophora moorcroftiana seeds after being crushed; extracting by using short-chain halogenated hydrocarbon as extracting solvent; filtering, and recovering the solvent; adding petroleum ether to dissolve, standing and crystallizing; and filtering and drying to obtain high-purity oxymatrine. The method has the advantages of less processes, simple device, convenience for operation and high oxymatrine purity.
Description
One, technical field
Patent of the present invention relates to from the Sophora moocroftiana(Wall seed separates the method for preparing Oxymatyine.
Two, technical background
Sophora moocroftiana(Wall (Sophora moorcroftiana) belongs to the perennial shrub of pulse family Sophora, is Qinghai-Tibet endemic plant, extensively distributes in the Tibet region, and checking winds and fixing drifting sand and reduce soil erosion for the locality has vital role.The Sophora moocroftiana(Wall seed is for use Tibetan medicine always simply; Hide title Ji watt; Bitter is cool in nature, and modern study is found wherein to contain abundant alkaloids composition, like Oxymatyine, matrine, Sophocarpidin, sophocarpine etc.; Wherein oxymatrine concentration is the high quality raw material as the preparation Oxymatyine far above kuh-seng content.
Oxymatyine (Oxymatrine) has another name called kurarinone, and the anti-hepatitis B virus effect is arranged, and can reduce the content of interior HBsAg of hepatitis B virus transgenic mice liver and HBcAg, has multiple patent medicine listing at present, is widely used in the treatment of hepatitis B.Utilizing the Sophora moocroftiana(Wall seed to prepare Oxymatyine technology has good economic worth, and can promote the protection and the exploitation of Tibet region Sophora moocroftiana(Wall.
About the existing report of the method that from Sophora moocroftiana(Wall, prepares Oxymatyine.CN1978446A discloses " a kind of technology of from Sophora moocroftiana(Wall, extracting Oxymatyine and matrine ", and this method is a raw material to pulverize Sophora moocroftiana(Wall seed or branch, extracts and concentrated extracting solution through alcohol heat reflux; The acidifying liquid concentrator filters and uses benzene class washing degreasing; After the water alkalization, use the extraction of halogenated alkane or benzene, concentrated extract obtains total alkali medicinal extract; Medicinal extract is used the acetone heating for dissolving; The cooling back adds ether leaves standstill, and separates out the Oxymatyine bullion, obtains Oxymatyine behind the acetone recrystallization.Xizang Jinke Technology Co., Ltd. in 2005 discloses in 1 scientific and technological achievement Sophora moocroftiana(Wall seed pulverizing back has been extracted with microwave under certain condition; Extraction liquid is through filtering, concentrate, liquid concentrator with 732 type cationic exchange coloums separate, must total alkaloids behind the concentrating under reduced pressure.Total alkaloids is dissolved in the minimum of chloroform, adds diethyl ether in 0-4 ℃, to spend the night, and throw out gets the method for Oxymatyine with acetone recrystallization.
Three, summary of the invention
Invention aims to provide a kind of method of from the Sophora moocroftiana(Wall seed, extracting Oxymatyine, and to be solved and technical problem is that flow process is extracted in the purity and the simplification that improve Oxymatyine.
The object of the invention realizes through following measure:
The present invention extracts the method for Oxymatyine from the Sophora moocroftiana(Wall seed, comprise each unit process of alkalization, extraction, dissolving, crystallization and aftertreatment:
Said alkalization is that the Sophora moocroftiana(Wall seed was pulverized 80 mesh sieves, adds the alkali lye formation alkalization system of pH value 9-11 then according to the ratio of solid-liquid ratio 1g:0.5 ~ 2mL, leaves standstill 0.5 ~ 2 hour;
Said extraction is in the alkalization system, to add the short chain halogenated alkane, and normal temperature stirs down and extracted 1 ~ 5 hour, filters and collects extracting solution, and the mass volume ratio of Sophora moocroftiana(Wall seed and short chain halogenated alkane is 1g:5 ~ 20mL;
Said dissolving is extracting solution to be revolved to steam to remove desolvate; Obtain oily mater; The sherwood oil that in oily mater, adds 5-12 times of volume; Left standstill crystallization 5-10 hour in-5 ~ 30 ℃ after the stirring and dissolving, filter and drying after obtain needle-like Oxymatyine bullion, the Oxymatyine bullion is dissolved in recrystallization promptly gets pure article in the methyl alcohol.
Alkali lye is selected from ammoniacal liquor, sodium hydroxide solution, potassium hydroxide solution, aqua calcis, sodium carbonate solution or solution of potassium carbonate described in the alkalization process; The addition of alkali lye is that every gram Sophora moocroftiana(Wall seed adds 0.5-2mL.
The addition of alkali lye is that every gram Sophora moocroftiana(Wall seed adds 1mL, and alkali lye left standstill 1 hour after adding.
The halogenated alkane of short chain described in the leaching process is selected from methylene dichloride, trichloromethane or 1, the 2-ethylene dichloride, and the mass volume ratio of Sophora moocroftiana(Wall seed and short chain halogenated alkane is 1g:10mL, extraction time is 2 hours.
The mass volume ratio of Sophora moocroftiana(Wall seed and sherwood oil is 1g:10mL in the dissolution process;
Tc is 15 ℃, and crystallization time is 8 hours.
Compared with present technology, beneficial effect of the present invention is embodied in:
The inventive method has only promptly obtained high-purity Oxymatyine through a step solvent extraction and an one step crystallizing; Use two kinds of organic solvents in the whole operation; Have the advantage that operation is few, equipment is simple, easy to operate, low production cost is convenient to realize the advantage of industrialization.
The purity of the Oxymatyine that the present invention extracts is greater than 97.0%.
Four, description of drawings
Fig. 1 is the high-efficient liquid phase chromatogram of the Oxymatyine product of the present invention's extraction.Adopt Kromasail C
18Chromatographic column, 250mm * 4.6mm, 5 μ m detect wavelength 220nm; Flow velocity: 1.0ml/min; Column temperature: 40 ℃; Moving phase: the triethylamine solution of methyl alcohol and mass concentration 0.06% is the mixing solutions of 55:45 formation by volume, phosphoric acid adjust pH to 7.0.
The Oxymatyine product infrared colour spectrogram that Fig. 2 extracts for the present invention.
The Oxymatyine product product mass spectrum that Fig. 3 extracts for the present invention.
The Oxymatyine product that Fig. 4 extracts for the present invention
13The C nuclear magnetic resonance spectrum.
The Oxymatyine product that Fig. 5 extracts for the present invention
1The H nuclear magnetic resonance spectrum.
Five, embodiment
To combine embodiment that the present invention is done further elaboration below, but the scope that the present invention requires to protect is not limited to following embodiment.
Embodiment 1:
Get Sophora moocroftiana(Wall seed 500g, pulverize and cross 80 mesh sieves and get the Sophora moocroftiana(Wall seed meal, the ammonia soln 500mL (solid-liquid ratio 1g:1mL) that adds mass concentration 50% left standstill 1 hour; The methylene dichloride normal temperature that adds 3000mL (solid-liquid ratio 1g:6mL) then stirred 1 hour down, suction filtration, and the methylene dichloride of same volume extracts once more; Merge extracted twice liquid, concentrating under reduced pressure removes to desolvate and obtains oily mater, in oily mater, adds the sherwood oil of 10 times of volumes; Stirring and dissolving, room temperature left standstill 10 hours, constantly separated out needle-like crystal; Filtration obtains the Oxymatyine bullion; The Oxymatyine bullion is dissolved in (50 ℃ of heating for dissolving) in the 5ml methyl alcohol, crystallisation by cooling, filter and drying after obtain needle-like crystal 5.2g.Detect through HPLC, be the Oxymatyine of purity 98.6%.
Embodiment 2:
Get Sophora moocroftiana(Wall seed 500g, pulverize and cross 80 mesh sieves and get the Sophora moocroftiana(Wall seed meal, add 0.1M sodium carbonate solution 500mL (solid-liquid ratio 1g:1mL) and left standstill 1 hour; The methylene dichloride normal temperature that adds 5000mL (solid-liquid ratio 1g:10mL) then stirred 2 hours down, suction filtration, and the methylene dichloride of same volume extracts once more; Merge extracted twice liquid, concentrating under reduced pressure removes to desolvate and obtains oily mater, in oily mater, adds the sherwood oil of 8 times of volumes; Left standstill under the stirring and dissolving, ice-water bath 10 hours, and constantly separated out needle-like crystal; Filtration obtains the Oxymatyine bullion; The Oxymatyine bullion is dissolved in (50 ℃ of heating for dissolving) in the 5ml methyl alcohol, crystallisation by cooling, filter and drying after obtain needle-like crystal 3.7g.Detect through HPLC, be the Oxymatyine of purity 97.2%.
Embodiment 3:
Get Sophora moocroftiana(Wall seed 500g, pulverize and cross 80 mesh sieves and get the Sophora moocroftiana(Wall seed meal, add 0.05M potassium hydroxide solution 1000mL (solid-liquid ratio 1g:2mL) and left standstill 2 hours; Add 1 of 3000mL (solid-liquid ratio 1g:6mL) then, 2-2 monochloroethane normal temperature stirred 1 hour down, suction filtration; 1 of same volume, 2-2 monochloroethane extracts once more, merges extracted twice liquid; Concentrating under reduced pressure removes to desolvate and obtains oily mater, in oily mater, adds the sherwood oil of 12 times of volumes, stirring and dissolving; Left standstill under the room temperature 10 hours, and constantly separated out needle-like crystal, filter and obtain the Oxymatyine bullion; The Oxymatyine bullion is dissolved in (50 ℃ of heating for dissolving) in the 5ml methyl alcohol, crystallisation by cooling, filter and drying after obtain needle-like crystal 4.4g.Detect through HPLC, be the Oxymatyine of purity 98.2%.
Claims (5)
1. a method of from the Sophora moocroftiana(Wall seed, extracting Oxymatyine comprises each unit process of alkalization, extraction, dissolving, crystallization and aftertreatment, it is characterized in that:
Said alkalization is that the Sophora moocroftiana(Wall seed was pulverized 80 mesh sieves, adds the alkali lye formation alkalization system of pH value 9-11 then according to the ratio of solid-liquid ratio 1g:0.5 ~ 2mL, leaves standstill 0.5 ~ 2 hour;
Said extraction is in the alkalization system, to add the short chain halogenated alkane, and normal temperature stirs down and extracted 1 ~ 5 hour, filters and collects extracting solution, and the mass volume ratio of Sophora moocroftiana(Wall seed and short chain halogenated alkane is 1g:5 ~ 20mL;
Said dissolving is extracting solution to be revolved to steam to remove desolvate; Obtain oily mater; The sherwood oil that in oily mater, adds 5-12 times of volume; Left standstill crystallization 5-10 hour in-5 ~ 30 ℃ after the stirring and dissolving, filter and drying after obtain the Oxymatyine bullion, the Oxymatyine bullion is dissolved in recrystallization in the methyl alcohol.
2. process for extracting according to claim 1 is characterized in that:
Alkali lye is selected from ammoniacal liquor, sodium hydroxide solution, potassium hydroxide solution, aqua calcis, sodium carbonate solution or solution of potassium carbonate described in the alkalization process; The addition of alkali lye is that every gram Sophora moocroftiana(Wall seed adds 0.5-2mL.
3. process for extracting according to claim 1 and 2 is characterized in that:
The addition of alkali lye is that every gram Sophora moocroftiana(Wall seed adds 1mL, and alkali lye left standstill 1 hour after adding.
4. process for extracting according to claim 1 is characterized in that:
The halogenated alkane of short chain described in the leaching process is selected from methylene dichloride, trichloromethane or 1, the 2-ethylene dichloride, and the mass volume ratio of Sophora moocroftiana(Wall seed and short chain halogenated alkane is 1g:10mL, extraction time is 2 hours.
5. process for extracting according to claim 1 is characterized in that:
The mass volume ratio of Sophora moocroftiana(Wall seed and sherwood oil is 1g:10mL in the dissolution process;
Tc is 15 ℃, and crystallization time is 8 hours.
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| CN201210270366.1A CN102766143B (en) | 2012-07-30 | 2012-07-30 | Method for extracting oxymatrine from Sophora moorcroftiana seeds |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111138433A (en) * | 2020-01-16 | 2020-05-12 | 西藏德康生物科技有限公司 | Method for extracting and purifying matrine from sophora moorcroftianain |
| CN111171032A (en) * | 2020-01-16 | 2020-05-19 | 西藏德康生物科技有限公司 | Raw material pretreatment method for extracting matrine from sophora moorcroftianain |
| CN111777610A (en) * | 2020-07-31 | 2020-10-16 | 西藏德康生物科技有限公司 | Method for separating and purifying oxymatrine from sophora moorcroftiana extract |
| CN111892600A (en) * | 2020-07-31 | 2020-11-06 | 西藏德康生物科技有限公司 | Method for extracting oxymatrine from sophora moorcroftianain roots and branches |
| CN112162054A (en) * | 2020-08-31 | 2021-01-01 | 中国农业科学院蜜蜂研究所 | Authenticity evaluation method of sophora moorcroftianain honey |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1978446A (en) * | 2005-11-29 | 2007-06-13 | 中国科学院地理科学与资源研究所 | Process for extracting oxymatrine and matrine from sophora moocroftiana |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1978446A (en) * | 2005-11-29 | 2007-06-13 | 中国科学院地理科学与资源研究所 | Process for extracting oxymatrine and matrine from sophora moocroftiana |
Non-Patent Citations (1)
| Title |
|---|
| 崔建芳等: "苦参等四种槐属植物药中生物碱的分析", 《中药通报》, vol. 11, no. 2, 28 February 1986 (1986-02-28) * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111138433A (en) * | 2020-01-16 | 2020-05-12 | 西藏德康生物科技有限公司 | Method for extracting and purifying matrine from sophora moorcroftianain |
| CN111171032A (en) * | 2020-01-16 | 2020-05-19 | 西藏德康生物科技有限公司 | Raw material pretreatment method for extracting matrine from sophora moorcroftianain |
| CN111777610A (en) * | 2020-07-31 | 2020-10-16 | 西藏德康生物科技有限公司 | Method for separating and purifying oxymatrine from sophora moorcroftiana extract |
| CN111892600A (en) * | 2020-07-31 | 2020-11-06 | 西藏德康生物科技有限公司 | Method for extracting oxymatrine from sophora moorcroftianain roots and branches |
| CN112162054A (en) * | 2020-08-31 | 2021-01-01 | 中国农业科学院蜜蜂研究所 | Authenticity evaluation method of sophora moorcroftianain honey |
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