CN101817856A - Method for extracting monotropein from medicinal Indianmulberry roots - Google Patents
Method for extracting monotropein from medicinal Indianmulberry roots Download PDFInfo
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- CN101817856A CN101817856A CN 201010150315 CN201010150315A CN101817856A CN 101817856 A CN101817856 A CN 101817856A CN 201010150315 CN201010150315 CN 201010150315 CN 201010150315 A CN201010150315 A CN 201010150315A CN 101817856 A CN101817856 A CN 101817856A
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Abstract
The invention relates to a method for monotropein from medicinal Indianmulberry roots. In the process, medicinal Indianmulberry roots are sued as raw material, ultrasonic extraction in ethanol is performed, extract is performed by condensation and is dispersed in water, absorption by polyamide resin is performed, ionic water is used to remove impurities, 30 percent ethanol is used for elution, a monotropein fraction is collected, condensation is performed, saturated dissolution in ethyl acetate is performed, the solution is stood for crystallization, and recrystallization is performed twice to obtain the product. When the method is used for producing the product, the cost is low, the yield is high and the purity is high.
Description
Technical field:
The present invention relates to a kind of method of from Root of Medicinal Indian mulberry, extracting monotropitoside, especially a kind of method that adopts supersound extraction, polyamide resin column absorption and recrystallization to prepare monotropitoside.
Background technology:
English name: Monotropein
Molecular formula: C
16H
22O
11
Molecular weight: 390.34
Composition source: be the herb extract of Pirolaceae plant Herba Pyrolae incarnatae; The dry root extract of Rubiaceae Root of Medicinal Indian mulberry platymiscium Root of Medicinal Indian mulberry Morinda officinalis How..
Function cures mainly: kidney-replenishing, strengthening the bones and muscles, wind-damp dispelling.It is soft to be used for cold infertile, the menoxenia of impotence and seminal emission, palace, few abdomen crymodynia, rheumatic arthralgia, muscles and bones impotence.Effects such as wind-damp dispelling, strengthening the bones and muscles, detoxifcation, hemostasis are arranged.
Contain carboxyl in the monotropitoside molecular structure and than poly-hydroxy isopolarity utmost point group, complex structure, polarity is big, is dissolved in vinyl acetic monomer, ethyl acetate, acetone, is soluble in ethanol, methyl alcohol, aqueous alcohol solutions and water.
Monotropitoside is a cyclenes ether ether terpene glucoside compounds, and for Root of Medicinal Indian mulberry is different from the characteristic component that this belongs to other plant, content is about 2% in the Root of Medicinal Indian mulberry leaf.The research of relevant monotropitoside is less, and all is to extract from Root of Medicinal Indian mulberry, and it is a lot of to need perfect place to also have.Be preferably 200 times of amount 80% methyl alcohol supersound extraction as extraction conditions in the fourth equality " Study on Extraction Method of monotropitoside in the Root of Medicinal Indian mulberry ", methyl alcohol toxicity is bigger, and consumption is many, in the production operator ' s health is had very big harm; Peng Duohua etc. " extraction separation of monotropitoside and assay thereof in the Root of Medicinal Indian mulberry " with the Root of Medicinal Indian mulberry after the drying and crushing through alcohol extracting, multiple organic solvent washing, last macroporous resin, stepwise elution, chromatography obtains product, this method step is many, organic solvent is wide in variety.
Summary of the invention:
The contriver tests through process optimization, has invented a kind of method for preparing monotropitoside from Root of Medicinal Indian mulberry.This technology is simple to operation, the product yield height, and production cost is low, and Root of Medicinal Indian mulberry can also extract Root of Medicinal Indian mulberry oil after extracting.
The present invention realizes by the following technical solutions:
A kind of method for preparing monotropitoside from Root of Medicinal Indian mulberry is characterized in that comprising following steps:
1) alcohol extracting: get the Root of Medicinal Indian mulberry raw material, pulverizing is 40 orders, adds raw material 8-10 and doubly measures (V/W) ethanol ultrasonic extraction, filter extracting solution, concentrated extracting solution, medicinal extract;
2) post separates: above-mentioned medicinal extract water-dispersion, by polyamide resin column absorption, use the deionized water removal of impurities, and 30% ethanol elution is got ethanol eluate;
3) recrystallization: with elutriant simmer down to medicinal extract, add ethyl acetate and heat saturated dissolving, leave standstill crystallization, leach crystallisate, recrystallization 2 times leaches cryodrying and promptly gets product.
Above-mentioned preparation method is characterized in that the step 1) alcohol concn is 45-55%, normal temperature supersound extraction 2 times.
Above-mentioned preparation method is characterized in that step 2) to disperse used water consumption be that the 4-6 of raw material doubly measures
Above-mentioned preparation method is characterized in that step 2) the deionized water flow velocity is 1BV/h, stop when colourless to effluent: 30% ethanol flow velocity is 2BV/h, stops when colourless to effluent.
Above-mentioned preparation method is characterized in that the crystallization for the first time of step 3) monotropitoside flow point is concentrated into the 1/6-1/10 of its volume, rearing crystal time 4-6 hour.
Above-mentioned preparation method is characterized in that step 3) recrystallization rearing crystal time 6-8 hour.
In sum, there is following advantage in the present invention: ultrasonic assisting makes solvent enter raw material inside very soon, and the extraction efficiency height do not have lot of energy consumption, so production cost is low; Find 30% ethanol after deliberation to the extraction effect of monotropitoside ground extractability near 80% methyl alcohol commonly used, but toxicity is littler, consumption is more economized, and separates in conjunction with polyamide resin and can isolate monotropitoside more up hill and dale; The solubleness of monotropitoside in ethyl acetate is relatively low, adopts ethyl acetate as the crystallization solvent, has reduced the danger in the operating process.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment:
The assay of monotropitoside adopts high performance liquid chromatography (with reference to fourth equality " HPLC measures the monotropitoside in the Root of Medicinal Indian mulberry " document) among the following embodiment, and concrete grammar is as follows:
High-efficient liquid phase chromatogram condition:
Chromatographic column: Kromalsil C
18Post (150mm * 4.6mm, 5m)
Moving phase: methyl alcohol-0.4% phosphate aqueous solution (5: 95 → 28.8: 71.2,15min)
Flow velocity: 1mlmin
-1
Detect wavelength: 231nm
Column temperature: 25 ℃
Embodiment 1:
Get Root of Medicinal Indian mulberry 200g (monotropitoside content 0.3%), pulverizing is 40 orders, adds 1.6L 45% ethanol, normal temperature supersound extraction 2 times, and united extraction liquid, ethanol is reclaimed in underpressure distillation, is condensed into the medicinal extract shape, with medicinal extract 800ml water-dispersion., colourless until effluent with deionized water earlier after filtering with 5L/h flow velocity eluting water solubility impurity by the absorption of 5L polyamide resin column, use 30% ethanol colourless until effluent again with 10L/h flow velocity wash-out monotropitoside, get ethanol eluate 16L.Ethanol eluate is evaporated to 2L places crystallization, growing the grain 4 hours leaches coarse crystallization thing 102g.The coarse crystallization thing heats saturated dissolving with ethyl acetate, places crystallization, and growing the grain 6 hours repeats crystallization 1 time with condition, leaches cryodrying, gets product 0.17g, content 95.2%.
Embodiment 2:
Get Root of Medicinal Indian mulberry 200g (monotropitoside content 0.3%), pulverizing is 40 orders, adds 1.6L 45% ethanol, normal temperature supersound extraction 2 times, and united extraction liquid, ethanol is reclaimed in underpressure distillation, is condensed into the medicinal extract shape, with medicinal extract 800ml water-dispersion., colourless until effluent with deionized water earlier after filtering with 5L/h flow velocity eluting water solubility impurity by the absorption of 5L polyamide resin column, use 30% ethanol colourless until effluent again with 10L/h flow velocity wash-out monotropitoside, get ethanol eluate 18L.Ethanol eluate is evaporated to 2L places crystallization, growing the grain 5 hours leaches coarse crystallization thing 103g.The coarse crystallization thing heats saturated dissolving with ethyl acetate, places crystallization, and growing the grain 6 hours repeats crystallization 1 time with condition, leaches cryodrying, gets product 0.16g, content 95.6%.
Embodiment 3:
Get Root of Medicinal Indian mulberry 200g (monotropitoside content 0.3%), pulverizing is 40 orders, adds 2L 50% ethanol, normal temperature supersound extraction 2 times, and united extraction liquid, ethanol is reclaimed in underpressure distillation, is condensed into the medicinal extract shape, with medicinal extract 1000ml water-dispersion., colourless until effluent with deionized water earlier after filtering with 5L/h flow velocity eluting water solubility impurity by the absorption of 5L polyamide resin column, use 30% ethanol colourless until effluent again with 10L/h flow velocity wash-out monotropitoside, get ethanol eluate 17L.Ethanol eluate is evaporated to 2L places crystallization, growing the grain 6 hours leaches coarse crystallization thing 105g.The coarse crystallization thing heats saturated dissolving with ethyl acetate, places crystallization, and growing the grain 7 hours repeats crystallization 1 time with condition, leaches cryodrying, gets product 0.17g, content 97.4%.
Embodiment 4:
Get Root of Medicinal Indian mulberry 200g (monotropitoside content 0.3%), pulverizing is 40 orders, adds 1.8L 50% ethanol, normal temperature supersound extraction 2 times, and united extraction liquid, ethanol is reclaimed in underpressure distillation, is condensed into the medicinal extract shape, with medicinal extract 1200ml water-dispersion., colourless until effluent with deionized water earlier after filtering with 5L/h flow velocity eluting water solubility impurity by the absorption of 5L polyamide resin column, use 30% ethanol colourless until effluent again with 10L/h flow velocity wash-out monotropitoside, get ethanol eluate 16L.Ethanol eluate is evaporated to 2L places crystallization, growing the grain 6 hours leaches coarse crystallization thing 111g.The coarse crystallization thing heats saturated dissolving with ethyl acetate, places crystallization, and growing the grain 8 hours repeats crystallization 1 time with condition, leaches cryodrying, gets product 0.16g, content 98.2%.
Claims (6)
1. method of extracting monotropitoside from Root of Medicinal Indian mulberry is characterized in that comprising following steps:
1) alcohol extracting: get the Root of Medicinal Indian mulberry raw material, pulverizing is 40 orders, adds raw material 8-10 and doubly measures (V/W) ethanol ultrasonic extraction, filter extracting solution, concentrated extracting solution, medicinal extract;
2) post separates: above-mentioned medicinal extract water-dispersion, by polyamide resin column absorption, use the deionized water removal of impurities, and 30% ethanol elution is got ethanol eluate;
3) recrystallization: with elutriant simmer down to medicinal extract, add ethyl acetate and heat saturated dissolving, leave standstill crystallization, leach crystallisate, recrystallization 2 times leaches cryodrying and promptly gets product.
2. preparation method as claimed in claim 1 is characterized in that the step 1) alcohol concn is 45-55%, normal temperature supersound extraction 2 times.
3. preparation method as claimed in claim 1 is characterized in that step 2) to disperse used water consumption be that the 4-6 of raw material doubly measures
4. preparation method as claimed in claim 1 is characterized in that step 2) the deionized water flow velocity is 1BV/h, stops when colourless to effluent; 30% ethanol flow velocity is 2BV/h, stops when colourless to effluent.
5. preparation method as claimed in claim 1 is characterized in that the crystallization for the first time of step 3) monotropitoside flow point is concentrated into the 1/6-1/10 of its volume, rearing crystal time 4-6 hour.
6. preparation method as claimed in claim 1 is characterized in that step 3) recrystallization rearing crystal time 6-8 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010150315 CN101817856A (en) | 2010-04-08 | 2010-04-08 | Method for extracting monotropein from medicinal Indianmulberry roots |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010150315 CN101817856A (en) | 2010-04-08 | 2010-04-08 | Method for extracting monotropein from medicinal Indianmulberry roots |
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| CN101817856A true CN101817856A (en) | 2010-09-01 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102649801A (en) * | 2011-02-25 | 2012-08-29 | 苏州宝泽堂医药科技有限公司 | Preparation method for monotropein monomer |
| CN102850417A (en) * | 2012-09-18 | 2013-01-02 | 成都瑞芬思生物科技有限公司 | Method for separating monotropein from pyrola |
| CN104311612A (en) * | 2014-09-30 | 2015-01-28 | 桂林三宝药业有限公司 | Method for extracting and separating monotropein from radix morindae officinalis |
| CN111548380A (en) * | 2020-06-10 | 2020-08-18 | 劲牌有限公司 | Preparation method of monotropein in morinda officinalis |
-
2010
- 2010-04-08 CN CN 201010150315 patent/CN101817856A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 《中南药学》 20081220 彭朵花等 巴戟天中水晶兰苷的提取分离及其含量测定 705-707页 1-6 , 第06期 2 * |
| 《中成药》 20070620 徐吉银等 巴戟天中水晶兰苷的提取方法研究 893-895页 1-6 , 第06期 2 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102649801A (en) * | 2011-02-25 | 2012-08-29 | 苏州宝泽堂医药科技有限公司 | Preparation method for monotropein monomer |
| CN102850417A (en) * | 2012-09-18 | 2013-01-02 | 成都瑞芬思生物科技有限公司 | Method for separating monotropein from pyrola |
| CN102850417B (en) * | 2012-09-18 | 2015-03-11 | 成都瑞芬思生物科技有限公司 | Method for separating monotropein from pyrola |
| CN104311612A (en) * | 2014-09-30 | 2015-01-28 | 桂林三宝药业有限公司 | Method for extracting and separating monotropein from radix morindae officinalis |
| CN111548380A (en) * | 2020-06-10 | 2020-08-18 | 劲牌有限公司 | Preparation method of monotropein in morinda officinalis |
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