CN102526134A - Preparation method of dipsacus total saponins and teasel saponins VI - Google Patents
Preparation method of dipsacus total saponins and teasel saponins VI Download PDFInfo
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- CN102526134A CN102526134A CN2010106038752A CN201010603875A CN102526134A CN 102526134 A CN102526134 A CN 102526134A CN 2010106038752 A CN2010106038752 A CN 2010106038752A CN 201010603875 A CN201010603875 A CN 201010603875A CN 102526134 A CN102526134 A CN 102526134A
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Abstract
The invention relates to a preparation method of dipsacus total saponins and teasel saponins VI. The preparation method comprises the following steps of: taking Chinese medical dipsacus as a raw material; crushing the raw material into coarse powder; degreasing with petroleum ether; drying and then extracting with hot water or 40-99% of ethanol for 2-4 times; recovering the ethanol; adding the obtained extract into a magnesium oxide column for carrying out chromatography; eluting with water-containing ethanol; concentrating the eluent until the eluent does not have ethanol taste; adding alkali to regulate the pH value; centrifuging; taking the supernatant, and concentrating and drying to obtain dipsacus total saponin extracts; separating the dipsacus total saponin extracts by adopting a high-speed counter-current chromatography; collecting fractions of teasel saponins VI by taking heptane-chloroform-ethanol-water as a solvent system; and concentrating, freeze-drying and crystallizing to obtain high-purity teasel saponins VI. The method provided by the invention can be used for simultaneously obtaining dipsacus total saponins and high-purity teasel saponins VI efficiently, simply and conveniently.
Description
Technical field:
The invention belongs to the preparation field of Radix Dipsaci saponin, particularly relate to the method for a kind of separation and purification on-off total saponin as well as and asperosaponin VI.
Background technology:
Radix Dipsaci is the dry root of Dipsacaceae plant Radix Dipsaci Dipsacus asper Wall.ex Henry.Beginning is stated from Shennong's Herbal, classifies as top grade.Bitter, hot, tepor.Return liver, kidney channel.Invigorating the liver and kidney, bone and muscle strengthening, continuous folding is hindered, and ends metrorrhagia.Be used for deficiency of the liver and kindey, soreness of the waist and knees, rheumatic arthralgia, injury from falling down, injury of tendon and muscle fracture, metrorrhagia, vaginal bleeding during pregnancy.Prepared RADIX DIPSACI with yellow rice wine is used for rheumatic arthralgia more, injury from falling down, injury of tendon and muscle fracture.Prepared RADIX DIPSACI with salt solution is used for soreness of the waist and knees more.Radix Dipsaci mainly contains triterpene and saponins compound thereof, the iridoid glycoside compounds, and alkaloid compound, phenolic acid compound, multiple composition such as flavone compound, known saponin component are its main effective ingredient.Liu Yong etc. are through the assay to total saponins in the Radix Dipsaci of the different places of production; The total saponins effective constituents of finding the wild Radix Dipsaci in Hefeng, Hubei all is higher than other areas; Up to 19.91%, find simultaneously Different Harvesting Time with the Frost's Descent in autumn the time Radix Dipsaci its total saponin content that falls to gather behind the Seedling be height.Tan Honggen etc. find that through experiment Hubei length is positive and Guanxian county, Sichuan asperosaponin VI content is the highest; The document record thinks that also the quality of Hubei and Sichuan Radix Dipsaci is better; Pharmacodynamic experiment also shows: asperosaponin VI has the effect of bone density improving; Using curing mainly with function of Radix Dipsaci " invigorating the liver and kidney, the bone of winnowing with a dustpan by force, continuous fractureing " with tcm clinical practice matches.Wu Feng Zhe etc. utilizes rat at body intestinal absorption experimental model; Adopt the HPLC method to measure asperosaponin VI and phenol red concentration in the intestinal circulation fluid; Asperosaponin VI rat is studied in body intestinal absorption characteristic, found that the coexistence composition in the asperosaponin VI extract can reduce its absorption; Its absorption pattern possibly be passive diffusion.
The method for extraction and purification of present domestic asperosaponin VI has: (1) lower alcohol or aqueous lower alcohol extraction filter reclaim under reduced pressure alcohol; Concentrate adjusting PH with base, macroporous resin column on the supernatant; Alkali liquor eluting, water elution, reuse alcohol eluting, peroxidating aluminum or decolorizing resin post or employing activated carbon decolorizing; Get bullion, further adopt column chromatography for separation or adopt opposed polarity solvent fractional extraction purification refine to make.(2) alcohol extraction, adjusting PH with base, water-saturated n-butanol extraction; The water that n-butanol layer reuse n-butyl alcohol is saturated extracts repeatedly; Get total saponins, be dissolved in water, fully precipitate through cooling or reduction solvent polarity to Radix Dipsaci saponin VI; To sedimentation and filtration or the centrifugal mother solution that wherein comprises of removing, will precipitate once more and repeat aforesaid operations with water dissolution and obtain Radix Dipsaci saponin VI monomer for 1-3 time.A large amount of organic solvents are grown, needed to use to this class methods complicated operation, extracting cycle.
Summary of the invention:
Technical scheme of the present invention provides the method for preparing of a kind of on-off total saponin as well as and asperosaponin VI.
The method for preparing of on-off total saponin as well as provided by the invention and asperosaponin VI, carry out according to the following steps:
1) extract: the Chinese medicine Radix Dipsaci is ground into coarse powder, use defat with petroleum ether, dry afterwards with hot water or 40-99% ethanol extraction 2-4 time, concentrating under reduced pressure gets extractum;
2) magnesium oxide column chromatography: gained extractum adds magnesium oxide chromatography post, and the aquiferous ethanol eluting is collected eluent and is concentrated into nothing alcohol flavor;
3) remove impurity: add alkali and regulate pH8-11, centrifugal, with supernatant concentration to do the on-off total saponin as well as extract;
4) high speed adverse current chromatogram separation and purification: the on-off total saponin as well as extract is separated with high-speed counter-current chromatograph, is solvent system with heptane-chloroform-alcohol-water, collects asperosaponin VI flow point, and concentrating under reduced pressure lyophilizing crystallization promptly obtains asperosaponin VI.
1) the described petroleum ether addition of step is a 2-3 times of medical material amount, volatilizes petroleum ether after ultrasonic degreasing 15-30 minute.
1) the described method for distilling of step is that supersound extraction or microwave-assisted extract, and extracts 40min-180min at every turn, is evaporated to the 1/5-1/15 of original volume.
2) the said magnesium oxide of step is a 100-150 order magnesium oxide, and the post blade diameter length ratio is 1: 5-20, eluant are 4-6BV cold water → 3-5BV50-80% ethanol.
4) step adopts high-speed countercurrent chromatography, and solvent system heptane-chloroform-alcohol-water volume ratio is: 2-5: 3-4: 6-7: 2-5, engine speed are 600-1500r/min, and the flow velocity that mobile phase pumps in the post is 0.5-5ml/min.
Good effect of the present invention is: adopt microwave or supersound extraction, the time spent is short, extraction efficiency is high; Adopt the magnesium oxide column chromatographic isolation and purification, reduced the separating difficulty of subsequent handling; The employing high-speed countercurrent chromatography separates, and high, pollution-free, quick, the big preparation amount of efficient separates asperosaponin VI, and the asperosaponin VI purity of acquisition can reach more than 98%.
The specific embodiment:
Below in conjunction with specific embodiment, the present invention is further set forth.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.
Embodiment 1:
Get Radix Dipsaci decoction pieces 1kg and be ground into coarse powder, with petroleum ether 2L ultrasonic degreasing 20min, volatilize remove petroleum ether after, using concentration of volume percent is 50% ethanol water 4L microwave extraction 3 times; Each 60min, extracting solution merge, are evaporated to 1000ml, add magnesium oxide column chromatography (100-150 order, post blade diameter length ratio 1: 10); With 5BV cold water → 5BV70% ethanol elution, collect 70% ethanol stream fluid successively, decompression recycling ethanol is to there not being the alcohol flavor; Add ammonia spirit while stirring and regulate pH to 8.5, leave standstill, the centrifugal supernatant that gets; Be concentrated into dried, pulverize on-off total saponin as well as powder 98.6g, content is 86%.
Adopt high speed adverse current chromatogram to separate on-off total saponin as well as; Under the room temperature with heptane-chloroform-alcohol-water 5: 3: 7 by volume: 5 place separatory funnel, and standing demix after the jolting is behind the ready to balance 30min; Get upper and lower phase respectively; To go up as immobile phase, following to mobile phase, take by weighing 100mg on-off total saponin as well as powder and be dissolved in the two phase liquid for use.Before the sample introduction, immobile phase is pumped in the chromatographic column, make to be full of whole pillar; The adjustment engine speed is 800r/min, with the flow velocity of 3.0ml/min mobile phase is pumped in the post, treat mobile phase from liquid outlet flow out and biphase set up dynamic equilibrium after; By injection valve sample solution is injected chromatographic system, simultaneously at fluid termination UV-detector, in the 212nm wavelength to the effluent continuous detecting; Compare with asperosaponin VI standard diagram, collect target component, obtain asperosaponin VI flow point; Carry out crystallization after concentrated freeze-dried, get asperosaponin VI, measure its purity through HPLC and reach more than 98%.
Embodiment 2:
Get Radix Dipsaci decoction pieces 1kg and be ground into coarse powder, with petroleum ether 3L ultrasonic degreasing 25min, volatilize remove petroleum ether after, with hot water 8L microwave extraction 4 times; Each 90min, extracting solution merge, are evaporated to 5000ml, add magnesium oxide column chromatography (100-150 order, post blade diameter length ratio 1: 5); With 4BV cold water → 3BV50% ethanol elution, collect 50% ethanol stream fluid successively, decompression recycling ethanol is to there not being the alcohol flavor; Add ammonia spirit while stirring and regulate pH to 8.0, leave standstill, the centrifugal supernatant that gets; Be concentrated into dried, pulverize on-off total saponin as well as powder 100.6g, content is 88%.
Adopt high speed adverse current chromatogram to separate on-off total saponin as well as; Under the room temperature with heptane-chloroform-alcohol-water 3: 4: 6 by volume: 4 place separatory funnel, and standing demix after the jolting is behind the ready to balance 30min; Get upper and lower phase respectively; To go up as immobile phase, following to mobile phase, take by weighing 100mg on-off total saponin as well as powder and be dissolved in the two phase liquid for use.Before the sample introduction, immobile phase is pumped in the chromatographic column, make to be full of whole pillar; The adjustment engine speed is 950r/min, with the flow velocity of 2.0ml/min mobile phase is pumped in the post, treat mobile phase from liquid outlet flow out and biphase set up dynamic equilibrium after; By injection valve sample solution is injected chromatographic system, simultaneously at fluid termination UV-detector, in the 212nm wavelength to the effluent continuous detecting; Compare with asperosaponin VI standard diagram, collect target component, obtain asperosaponin VI flow point; Carry out crystallization after concentrated freeze-dried, get asperosaponin VI, measure its purity through HPLC and reach more than 98%.
Embodiment 3:
Get Radix Dipsaci decoction pieces 1kg and be ground into coarse powder, with petroleum ether 3L ultrasonic degreasing 30min, volatilize remove petroleum ether after, using concentration of volume percent is 70% ethanol water 5L microwave extraction 2 times; Each 180min, extracting solution merge, are evaporated to 2000ml, add magnesium oxide column chromatography (100-150 order, post blade diameter length ratio 1: 15); With 6BV cold water → 5BV80% ethanol elution, collect 80% ethanol stream fluid successively, decompression recycling ethanol is to there not being the alcohol flavor; Add ammonia spirit while stirring and regulate pH to 9.0, leave standstill, the centrifugal supernatant that gets; Be concentrated into dried, pulverize on-off total saponin as well as powder 109.4g, content is 87%.
Adopt high speed adverse current chromatogram to separate on-off total saponin as well as; Under the room temperature with heptane-chloroform-alcohol-water 4: 3: 7 by volume: 2 place separatory funnel, and standing demix after the jolting is behind the ready to balance 30min; Get upper and lower phase respectively; To go up as immobile phase, following to mobile phase, take by weighing 100mg on-off total saponin as well as powder and be dissolved in the two phase liquid for use.Before the sample introduction, immobile phase is pumped in the chromatographic column, make to be full of whole pillar; The adjustment engine speed is 1000r/min, with the flow velocity of 3.5ml/min mobile phase is pumped in the post, treat mobile phase from liquid outlet flow out and biphase set up dynamic equilibrium after; By injection valve sample solution is injected chromatographic system, simultaneously at fluid termination UV-detector, in the 212nm wavelength to the effluent continuous detecting; Compare with asperosaponin VI standard diagram, collect target component, obtain asperosaponin VI flow point; Carry out crystallization after concentrated freeze-dried, get asperosaponin VI, measure its purity through HPLC and reach more than 98%.
Embodiment 4:
Get Radix Dipsaci decoction pieces 1kg and be ground into coarse powder, with petroleum ether 2L ultrasonic degreasing 15min, volatilize remove petroleum ether after, using concentration of volume percent is 90% ethanol water 4L microwave extraction 3 times; Each 120min, extracting solution merge, are evaporated to 800ml, add magnesium oxide column chromatography (100-150 order, post blade diameter length ratio 1: 20); With 5BV cold water → 4BV80% ethanol elution, collect 80% ethanol stream fluid successively, decompression recycling ethanol is to there not being the alcohol flavor; Add ammonia spirit while stirring and regulate pH to 9.5, leave standstill, the centrifugal supernatant that gets; Be concentrated into dried, pulverize on-off total saponin as well as powder 97.1g, content is 90%.
Adopt high speed adverse current chromatogram to separate on-off total saponin as well as; Under the room temperature with heptane-chloroform-alcohol-water 2: 4: 6 by volume: 3 place separatory funnel, and standing demix after the jolting is behind the ready to balance 30min; Get upper and lower phase respectively; To go up as immobile phase, following to mobile phase, take by weighing 100mg on-off total saponin as well as powder and be dissolved in the two phase liquid for use.Before the sample introduction, immobile phase is pumped in the chromatographic column, make to be full of whole pillar; The adjustment engine speed is 1200r/min, with the flow velocity of 5.0ml/min mobile phase is pumped in the post, treat mobile phase from liquid outlet flow out and biphase set up dynamic equilibrium after; By injection valve sample solution is injected chromatographic system, simultaneously at fluid termination UV-detector, in the 212nm wavelength to the effluent continuous detecting; Compare with asperosaponin VI standard diagram, collect target component, obtain asperosaponin VI flow point; Carry out crystallization after concentrated freeze-dried, get asperosaponin VI, measure its purity through HPLC and reach more than 98%.
Claims (5)
1. the method for preparing of on-off total saponin as well as and asperosaponin VI is characterized in that carrying out according to the following steps:
1) extract: the Chinese medicine Radix Dipsaci is ground into coarse powder, use defat with petroleum ether, dry afterwards with hot water or 40-99% ethanol extraction 2-4 time, concentrating under reduced pressure gets extractum;
2) magnesium oxide column chromatography: gained extractum adds magnesium oxide chromatography post, and the aquiferous ethanol eluting is collected eluent and is concentrated into nothing alcohol flavor;
3) remove impurity: add alkali and regulate pH8-11, centrifugal, with supernatant concentration to do the on-off total saponin as well as extract;
4) high speed adverse current chromatogram separation and purification: the on-off total saponin as well as extract is separated with high-speed counter-current chromatograph, is solvent system with heptane-chloroform-alcohol-water, collects asperosaponin VI flow point, and concentrating under reduced pressure lyophilizing crystallization promptly obtains asperosaponin VI.
2. the method for preparing of on-off total saponin as well as according to claim 1 and Radix Dipsaci total saponins VI is characterized in that: 1) the described petroleum ether addition of step is a 2-3 times of medical material amount, volatilizes petroleum ether after ultrasonic degreasing 15-30 minute.
3. the method for preparing of on-off total saponin as well as according to claim 1 and Radix Dipsaci total saponins VI; It is characterized in that: 1) the described method for distilling of step is that supersound extraction or microwave-assisted extract; Extract 40min-180min at every turn, be evaporated to the 1/5-1/15 of original volume.
4. the method for preparing of on-off total saponin as well as according to claim 1 and Radix Dipsaci total saponins VI is characterized in that: 2) the said magnesium oxide of step is a 100-150 order magnesium oxide, and the post blade diameter length ratio is 1: 5-20, eluant are 4-6BV cold water → 3-5BV50-80% ethanol.
5. the method for preparing of on-off total saponin as well as according to claim 1 and Radix Dipsaci total saponins VI; It is characterized in that: 4) step adopts high-speed countercurrent chromatography; Solvent system heptane-chloroform-alcohol-water volume ratio is: 2-5: 3-4: 6-7: 2-5; Engine speed is 600-1500r/min, and the flow velocity that mobile phase pumps in the post is 0.5-5ml/min.
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Cited By (4)
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| CN102924545A (en) * | 2012-11-13 | 2013-02-13 | 杨中林 | Enrichment and purifying method of akebiaquinata saponin D |
| CN109575101A (en) * | 2018-12-28 | 2019-04-05 | 湖南津湘制药有限公司 | A kind of highly effective extraction method of teasel root saponin(e VI |
| CN112156101A (en) * | 2020-09-18 | 2021-01-01 | 成都体育学院 | Application of dipsacus asperoides VI in preparation of medicine for treating tendon injury |
| CN113336810A (en) * | 2021-01-15 | 2021-09-03 | 广州博济医药生物技术股份有限公司 | Method for extracting and purifying teasel root saponin VI with high bioavailability |
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| CN109575101A (en) * | 2018-12-28 | 2019-04-05 | 湖南津湘制药有限公司 | A kind of highly effective extraction method of teasel root saponin(e VI |
| CN112156101A (en) * | 2020-09-18 | 2021-01-01 | 成都体育学院 | Application of dipsacus asperoides VI in preparation of medicine for treating tendon injury |
| CN113336810A (en) * | 2021-01-15 | 2021-09-03 | 广州博济医药生物技术股份有限公司 | Method for extracting and purifying teasel root saponin VI with high bioavailability |
| CN113336810B (en) * | 2021-01-15 | 2023-06-02 | 博济医药科技股份有限公司 | Extraction and purification method of dipsacus saponin VI with high bioavailability |
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Application publication date: 20120704 |