CN102391350A - Method for purifying polygalasaponin F - Google Patents
Method for purifying polygalasaponin F Download PDFInfo
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- CN102391350A CN102391350A CN2011103038863A CN201110303886A CN102391350A CN 102391350 A CN102391350 A CN 102391350A CN 2011103038863 A CN2011103038863 A CN 2011103038863A CN 201110303886 A CN201110303886 A CN 201110303886A CN 102391350 A CN102391350 A CN 102391350A
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- extract
- polygalasaponin
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- purifying
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention discloses a method for purifying polygalasaponin F. The method comprises the following steps of: i, crushing the polygalasaponin F serving as a medicinal material into 60 to 80 meshes, adding the medicinal material powder into a supercritical extraction kettle, performing supercritical extraction for 2 to 3 hours under the pressure of 15 to 25MPa and at the temperature of between 40 and 60 DEG C by introducing liquid CO2 and entrainer, resolving the extract under the pressure of 5 to 10MPa and at the temperature of between 50 and 60 DEG C, discharging the raw material residue, performing microwave extraction by adding 70 to 90 percent ethanol solution, concentrating the extract, adding the concentrate into macroporous resin for adsorption, performing elution by taking 40 to 70 percent ethanol solution in an amount which is 3 to 7 times weight of the concentrate, collecting the elute, and concentrating the elute to obtain an extract; and ii, purifying the extract by adopting high-speed countercurrent chromatography, detecting the purified extract by adopting an evaporative light scattering detector, collecting the target component, reclaiming the reagent, performing reduced pressure drying, and thus obtaining the polygalasaponin F. The method for purifying the polygalasaponin F is short in production period, high in efficiency, low in pollution and suitable for industrialized production.
Description
Technical field
The present invention relates to oneself method of purification of a kind of Japanese polygala saponin, particularly relate to oneself efficient method for rapidly purifying of a kind of Japanese polygala saponin.
Background technology
Japanese Milkwort Herb is the milk wort Japanese Milkwort Herb
Polygala jaPonicaHoutt. dry herb.Be cinnabar grass, golden key, melon seeds grass again, hang rice grass, polygala japonica houtt., Herbof Smallflower Milkwort.Traditional medicine thinks that the Japanese Milkwort Herb nature and flavor are hot, bitter, has expelling phlegm for arresting cough, activating blood circulation and reducing swelling, effects such as detoxifcation pain relieving.Be used for coughing with a lot of sputum, swelling and pain in the throat; Control wound outward, treat the sore furuncle, snake bite and insect sting.Modern study shows, contains multiple functional ingredient such as saponins, Flavonoid substances in the Japanese Milkwort Herb, have hypoglycemic, anti-inflammatory is calm and antitumor action.
Japanese polygala saponin oneself (Polygalasaponin F) be a kind of from Japanese Milkwort Herb isolated triterpenes saponin(e, molecular formula C53H86O23, have hypoglycemic, anti-inflammatory is calm and antitumor action, also is the index property composition of weighing the Japanese Milkwort Herb quality of medicinal material.
Through literature search, oneself method of purification Japanese polygala saponin adopts alcohol reflux more, goes up macroporous resin adsorption behind the extracting solution reconcentration, and elutriant subtracts institute's back silicagel column and sends out and separate or own through the high purity Japanese polygala saponin of gel column, preparation liquid phase separation system again.Like patent (application number: 200410089313.5) " Japanese polygala saponin kind compound and aglycon, total saponins and total sapogenin and the application in medicine thereof " and document " Japanese Milkwort Herb effective part group anti-inflammatory action Mechanism Study ".Mostly these methods are complicated operation, and especially in silicagel column and gel column sepn process, reagent dosage is big, and the sample yield is low, and the cycle is longer, especially low at the amplification process repetition rate, and the Personnel Skill Levels is had relatively high expectations, and cause that the confession amount is little, price is high.
Summary of the invention
The objective of the invention is to overcome the defective and the deficiency of prior art, provide a kind of Japanese polygala saponin oneself method of purification, method is simple to operate, and efficient is high.
The objective of the invention is to realize through following technical scheme:
Oneself method of purification of a kind of Japanese polygala saponin is characterized in that following steps:
I gets Japanese Milkwort Herb pulverizing medicinal materials 60-80 order, adds in the supercritical extraction reactor, under extracting pressure 15-25MPa, temperature 40-60 ℃ condition; Fed liquid CO 2 and entrainment agent supercritical extraction 2-3 hour, and, resolved extract for temperature 50-60 ℃ at pressure 5-10MPa; The raw material residue is emitted and is added 70-90% ethanolic soln microwave extraction; Extracting solution concentrate to add in the macroporous resin and adsorbs, and gets 3-7 and doubly measures 40-70% ethanolic soln wash-out, collect elutriant concentrate medicinal extract;
Ii adopts the high speed adverse current chromatogram purifying to above-mentioned medicinal extract, and light scattering detector detects, and collects target component, reclaims reagent, and drying under reduced pressure promptly gets.
A kind of in the optional methyl alcohol of described entrainment agent, ethanol, the acetoneand ethyl acetate, consumption is that the 1-3 of raw material doubly measures
A kind of among the optional NK-9 of described macroporous resin, ADS-21 and the HPD417.
The optional ETHYLE ACETATE of the isolating solvent systems of described high speed adverse current chromatogram, butanols, first alcohol and water quaternary solvent systems, blending ratio 4-10:1-3:1-2:5-10 gets the phase that fixes mutually, does moving phase down mutually.
The optional ETHYLE ACETATE of the isolating solvent systems of described high speed adverse current chromatogram, propyl carbinol and water ternary solvent system, blending ratio 3-10:1-2:5-15 gets the phase that fixes mutually, does moving phase down mutually.
Technical superiority of the present invention has:
1. method has adopted the supercritical CO 2 extracting impurities, because oneself molecular weight of Japanese polygala saponin is big, be difficult for being extracted out, and small molecules and low polar material especially has being extracted out more easily of entrainment agent, and this removal of impurities mode is easy and simple to handle, and the cycle is shorter.
2. method has adopted the high-speed countercurrent chromatography purifying, and method is simple and easy to operate, and solvent load is little, the sample free of losses, and preparation amount is big, can prepare continuously, and also pollution-free.
Embodiment
To combine embodiment to further specify the present invention below.
Embodiment 1:
Japanese Milkwort Herb pulverizing medicinal materials 60 orders are got 1kg and are added in the supercritical extraction reactor, feed liquid CO 2; Be arranged on 50 ℃ of extracting pressure 20MPa, temperature, reach above-mentioned parameter after, adjustment liquid CO 2 flow velocity is 20kg/h; Feed anhydrous methanol 1L/h simultaneously; Dynamic extraction 3 hours, at pressure 5MPa, temperature transfers part to resolve extract down for 50 ℃.The raw material residue is emitted and was added 20L70% ethanolic soln microwave extraction 30 minutes, extracts 2 times, and the extracting solution concentrating under reduced pressure adds the suitable quantity of water dilution, adds in the 300gNK-9 macroporous resin and adsorbs, and gets 3 times of amount 70% ethanolic soln wash-outs, collects the elutriant concentrating under reduced pressure and gets medicinal extract 12g.
Get ETHYLE ACETATE, butanols, methyl alcohol and water solvent, 4:1:1:5 mixes in proportion, and fully after the layering, getting fixes mutually fills with the high speed adverse current chromatogram pipe, rotates main frame 800rpm; Pump into down and do moving phase mutually, treat running balance after, flow velocity is adjusted into 2ml/min, dissolves medicinal extract with moving phase simultaneously; By the sampling valve sample introduction, target component is collected in the online detection of light scattering detector, continuously preparation; Reclaim reagent, drying under reduced pressure gets the own 3g of white powder Japanese polygala saponin, through detecting content 95.2%.
Embodiment 2:
Japanese Milkwort Herb pulverizing medicinal materials 80 orders are got 1kg and are added in the supercritical extraction reactor, feed liquid CO 2; Be arranged on 50 ℃ of extracting pressure 25MPa, temperature, reach above-mentioned parameter after, adjustment liquid CO 2 flow velocity is 20kg/h; Feed anhydrous propanone 300ml/h simultaneously; Dynamic extraction 3 hours, at pressure 8MPa, temperature transfers part to resolve extract down for 50 ℃.The raw material residue is emitted and was added 60L90% ethanolic soln microwave extraction 30 minutes; Extract 3 times, the extracting solution concentrating under reduced pressure adds the suitable quantity of water dilution, adds in the 400g ADS-21 macroporous resin and adsorbs; Get 5 times of amount 50% ethanolic soln wash-outs, collect the elutriant concentrating under reduced pressure and get medicinal extract 9g.
Get ETHYLE ACETATE, butanols, methyl alcohol and water solvent, 5:1:1:7 mixes in proportion, and fully after the layering, getting fixes mutually fills with the high speed adverse current chromatogram pipe, rotates main frame 900rpm; Pump into down and do moving phase mutually, treat running balance after, flow velocity is adjusted into 3ml/min, dissolves medicinal extract with moving phase simultaneously; By the sampling valve sample introduction, target component is collected in the online detection of light scattering detector, continuously preparation; Reclaim reagent, drying under reduced pressure gets the own 3.4g of white powder Japanese polygala saponin, through detecting content 98.5%.
Embodiment 3:
Japanese Milkwort Herb pulverizing medicinal materials 60 orders are got 1kg and are added in the supercritical extraction reactor, feed liquid CO 2; Be arranged on 60 ℃ of extracting pressure 15MPa, temperature, reach above-mentioned parameter after, adjustment liquid CO 2 flow velocity is 20kg/h; Feed 95% ethanol 1L/h simultaneously; Dynamic extraction 3 hours, at pressure 5MPa, temperature transfers part to resolve extract down for 60 ℃.The raw material residue is emitted and was added 20L70% ethanolic soln microwave extraction 30 minutes; Extract 2 times, the extracting solution concentrating under reduced pressure adds the suitable quantity of water dilution, adds in the 350g HPD417 macroporous resin and adsorbs; Get 7 times of amount 40% ethanolic soln wash-outs, collect the elutriant concentrating under reduced pressure and get medicinal extract 14g.
Get ETHYLE ACETATE, propyl carbinol and water solvent, 4:1:5 mixes in proportion, and fully after the layering, getting fixes mutually fills with the high speed adverse current chromatogram pipe, rotates main frame 700rpm; Pump into down and do moving phase mutually, treat running balance after, flow velocity is adjusted into 1ml/min, dissolves medicinal extract with moving phase simultaneously; By the sampling valve sample introduction, target component is collected in the online detection of light scattering detector, continuously preparation; Reclaim reagent, drying under reduced pressure gets the own 3.7g of white powder Japanese polygala saponin, through detecting content 97.5%.
Claims (5)
1. oneself method of purification of a Japanese polygala saponin is characterized in that following steps:
I gets Japanese Milkwort Herb pulverizing medicinal materials 60-80 order, adds in the supercritical extraction reactor, under extracting pressure 15-25MPa, temperature 40-60 ℃ condition; Fed liquid CO 2 and entrainment agent supercritical extraction 2-3 hour, and, resolved extract for temperature 50-60 ℃ at pressure 5-10MPa; The raw material residue is emitted and is added 70-90% ethanolic soln microwave extraction; Extracting solution concentrates the back and adds in the macroporous resin and adsorbs, and gets 3-7 and doubly measures 40-70% ethanolic soln wash-out, collect elutriant concentrate medicinal extract;
Ii adopts the high speed adverse current chromatogram purifying to above-mentioned medicinal extract, and light scattering detector detects, and collects target component, reclaims reagent, and drying under reduced pressure promptly gets.
2. oneself method of purification of Japanese polygala saponin according to claim 1 is characterized in that in the optional methyl alcohol of the entrainment agent described in the step I, ethanol, the acetoneand ethyl acetate a kind ofly, and consumption is that the 1-3 of raw material doubly measures.
3. oneself method of purification of Japanese polygala saponin according to claim 1 is characterized in that a kind of among the optional NK-9 of the macroporous resin described in the step I, ADS-21 and the HPD417.
4. oneself method of purification of Japanese polygala saponin according to claim 1; It is characterized in that the optional ETHYLE ACETATE of the isolating solvent systems of the high speed adverse current chromatogram described in the step I i, butanols, first alcohol and water quaternary solvent systems; Blending ratio 4-10:1-3:1-2:5-10; Get the phase that fixes mutually, do moving phase down mutually.
5. oneself method of purification of Japanese polygala saponin according to claim 1; It is characterized in that the optional ETHYLE ACETATE of the isolating solvent systems of the high speed adverse current chromatogram described in the step I i, propyl carbinol and water ternary solvent system; Blending ratio 3-10:1-2:5-15; Get the phase that fixes mutually, do moving phase down mutually.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103038863A CN102391350A (en) | 2011-10-10 | 2011-10-10 | Method for purifying polygalasaponin F |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103038863A CN102391350A (en) | 2011-10-10 | 2011-10-10 | Method for purifying polygalasaponin F |
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| CN102391350A true CN102391350A (en) | 2012-03-28 |
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| CN2011103038863A Pending CN102391350A (en) | 2011-10-10 | 2011-10-10 | Method for purifying polygalasaponin F |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20170076429A (en) * | 2015-12-24 | 2017-07-04 | 주식회사 엘지생활건강 | Composition for improving skin conditions comprising Polygalasaponin F |
| CN108158996A (en) * | 2018-03-19 | 2018-06-15 | 董宁霞 | A kind of Polygalasaponin F spray and preparation method thereof |
| CN108619906A (en) * | 2018-05-31 | 2018-10-09 | 李兵峰 | Environmentally friendly finishing eliminating smell agent and preparation method thereof |
| CN111690470A (en) * | 2020-07-10 | 2020-09-22 | 赵立红 | Natural green plant detergent and preparation method thereof |
| CN115212252A (en) * | 2022-08-18 | 2022-10-21 | 云南省中医医院(云南中医药大学第一附属医院) | Application of Va drug Nierone in preparation of drugs for treating cerebral infarction |
-
2011
- 2011-10-10 CN CN2011103038863A patent/CN102391350A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20170076429A (en) * | 2015-12-24 | 2017-07-04 | 주식회사 엘지생활건강 | Composition for improving skin conditions comprising Polygalasaponin F |
| KR102503107B1 (en) | 2015-12-24 | 2023-02-22 | 주식회사 엘지생활건강 | Composition for improving skin conditions comprising Polygalasaponin F |
| CN108158996A (en) * | 2018-03-19 | 2018-06-15 | 董宁霞 | A kind of Polygalasaponin F spray and preparation method thereof |
| CN108158996B (en) * | 2018-03-19 | 2020-06-02 | 董宁霞 | A fructus Trichosanthis and radix Polygalae saponin spray and its preparation method |
| CN108619906A (en) * | 2018-05-31 | 2018-10-09 | 李兵峰 | Environmentally friendly finishing eliminating smell agent and preparation method thereof |
| CN108619906B (en) * | 2018-05-31 | 2021-04-06 | 杭州康嘻环保科技有限公司 | Environment-friendly deodorant for decoration and preparation method thereof |
| CN111690470A (en) * | 2020-07-10 | 2020-09-22 | 赵立红 | Natural green plant detergent and preparation method thereof |
| CN115212252A (en) * | 2022-08-18 | 2022-10-21 | 云南省中医医院(云南中医药大学第一附属医院) | Application of Va drug Nierone in preparation of drugs for treating cerebral infarction |
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Application publication date: 20120328 |