CN107722100A - The purification process of ginsenoside Rg1 - Google Patents
The purification process of ginsenoside Rg1 Download PDFInfo
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- CN107722100A CN107722100A CN201711034686.6A CN201711034686A CN107722100A CN 107722100 A CN107722100 A CN 107722100A CN 201711034686 A CN201711034686 A CN 201711034686A CN 107722100 A CN107722100 A CN 107722100A
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Abstract
The invention belongs to technical field of extraction of Chinese traditional medicine, and in particular to a kind of purification process of ginsenoside Rg1.Arasaponin is dissolved in 95% ethanol, obtains solution；Neutral alumina aluminium powder is weighed, post is filled after being soaked with 95% ethanol；By the solution loading of gained；With 95% alcohol flushing, then with 85% alcohol flushing；The eluent rich in ginsenoside Rg1 is collected, is evaporated to obtain ginsenoside Rg1's crude product；By ginsenoside Rg1's dissolving crude product of gained in n-butanol phase, then extracted with isometric aqueous phase, collect n-butanol phase, be evaporated to obtain ginsenoside Rg1.The present invention have found a kind of filler and purification process cheap and easy to get for being suitable for ginsenoside Rg1's purifying, effectively reduce production cost.
Description
Technical field
The invention belongs to technical field of extraction of Chinese traditional medicine, and in particular to a kind of purification process of ginsenoside Rg1.
Background technology
Pseudo-ginseng is the dry root or rhizome of Araliaceae, is China's rare medicinal herbs, its principle active component is saponins
Compound, mainly including notoginsenoside R, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1 and ginsenoside Rd etc..Often
For it is promoting blood circulation and removing blood stasis, promote blood circulation active, have pharmacological action to hyperlipidemia, hypercoagulable blood, hypertension, while there is anti-cardiac muscle to lack
Blood, antiatherosclerosis, antithrombotic, anti-cardiac-cerebral ischemia etc. act on.
Ginsenoside Rg1 has good pharmacological activity, has treatment cardiovascular and cerebrovascular disease, antithrombotic, anti-fibrosis, controls
Treat senile dementia, improve the effect such as immunity, vasodilator, antifatigue and adjuvant therapy of tumors.
The separation that traditional handicraft carries out ginsenoside Rg1 using silica gel column chromatography is prepared, it is necessary to use substantial amounts of methanol, chlorine
The organic solvent such as imitative, dichloromethane and ethyl acetate, not only wastes time and energy, efficiency is low, operating difficulties, production cost are high, and
And environmental pollution is easily caused, the shortcomings of inconvenience of the solvent that uses recycles.
Reported in patent CN101463061B and patent CN101575357B and utilize reversed-phase silica gel column chromatography or glucan
The method that gel filtration chromatography separates ginsenoside Rg1.The eluant, eluent that this method uses is ethanol-water system, is avoided organic molten
The use of agent, but the filler used is C18 reversed-phase bonded silicas or sephadex, it is expensive, be not suitable for industrialized production.
Reported in patent CN105801656A and utilize monodisperse polymer silica gel column chromatography separation ginsenoside Rg1, ginseng
The method of the saponin(es such as saponin(e Re.The eluant, eluent that this method uses is ethanol-water system, avoids the use of organic solvent, but is made
Filler is monodisperse polymer silica gel, expensive, is not suitable for large-scale industrial production.
The content of the invention
It is simple and easy, be suitable for industrial metaplasia it is an object of the invention to provide a kind of purification process of ginsenoside Rg1
Produce, reduce production cost.
The purification process of ginsenoside Rg1 of the present invention, step are as follows：
(1) arasaponin is dissolved in 95% ethanol, obtains solution；
(2) neutral alumina aluminium powder is weighed, post is filled after being soaked with 95% ethanol；
(3) by step (1) obtained by solution loading；
(4) with 95% alcohol flushing, then with 85% alcohol flushing；
(5) eluent rich in ginsenoside Rg1 is collected, is evaporated to obtain ginsenoside Rg1's crude product；
(6) by ginsenoside Rg1's dissolving crude product obtained by step (5) in n-butanol phase, then extracted with isometric aqueous phase
Take, collect n-butanol phase, be evaporated to obtain ginsenoside Rg1.
The proportioning of arasaponin and 95% ethanol is 1 in step (1)：5-1：10, arasaponin is in terms of g, 95% second
Alcohol is in terms of mL.
The mesh number of neutral alumina aluminium powder is 80-400 mesh in step (2).
The proportioning of neutral alumina aluminium powder and 95% ethanol is 1 in step (2)：2-1：5, neutral alumina aluminium powder in terms of g,
95% ethanol is in terms of mL.
The ratio of the quality of arasaponin and column volume is 1 in step (2)：50, quality is in terms of g, and column volume is in terms of ml.
The flow of 95% alcohol flushing is 4-6BV in step (4).
The flow of 85% alcohol flushing is 10-12BV in step (4).
The proportioning of ginsenoside Rg1's crude product and n-butanol phase is 1 in step (6)：15-1：30, ginsenoside Rg1's crude product with
G is counted, and n-butanol is mutually in terms of mL.
Extraction times are 4 times in step (6).
The present invention compared with prior art, has the advantages that：
The defects of for prior art, the present invention have found it is a kind of be suitable for ginsenoside Rg1 purifying it is cheap and easy to get
Filler and purification process, effectively reduce production cost.
Embodiment
The present invention is described further with reference to embodiments.
Embodiment 1
Arasaponin 5.0g is dissolved in the ethanol of 40ml 95%；The neutral alumina aluminium powder of 80-160 mesh is weighed, is used
Post, column volume 250ml are filled after the immersion of 95% ethanol；By the ethanol solution loading of arasaponin, with 95% alcohol flushing
4BV, then with 85% alcohol flushing 10BV；The eluent rich in ginsenoside Rg1 is collected, is evaporated to obtain ginsenoside Rg1's crude product；
The proportioning of ginsenoside Rg1's crude product n-Butanol soluble, ginsenoside crude product (g) and n-butanol (mL) is 1：30, then use etc.
Volume aqueous phase extracts 4 times, collects n-butanol phase, is evaporated to obtain ginsenoside Rg1 0.94g；The purity of ginsenoside Rg1 is
98.5%.
Embodiment 2
Arasaponin 5.0g is dissolved in the ethanol of 50ml 95%；The neutral alumina aluminium powder of 80-160 mesh is weighed, is used
Post, column volume 250ml are filled after the immersion of 95% ethanol；By the ethanol solution loading of arasaponin, with 95% alcohol flushing
6BV, then with 85% alcohol flushing 12BV；The eluent rich in ginsenoside Rg1 is collected, is evaporated to obtain ginsenoside Rg1's crude product；
The proportioning of ginsenoside Rg1's crude product n-Butanol soluble, ginsenoside crude product (g) and n-butanol (mL) is 1：15, then use etc.
Volume aqueous phase extracts 4 times, collects n-butanol phase, is evaporated to obtain ginsenoside Rg1 0.98g；The purity of ginsenoside Rg1 is
98.1%.
Embodiment 3
Arasaponin 5.0g is dissolved in the ethanol of 40ml 95%；The neutral alumina aluminium powder of 300-400 mesh is weighed,
Post, column volume 250ml are filled after being soaked with 95% ethanol；By the ethanol solution loading of arasaponin, with 95% alcohol flushing
4BV, then with 85% alcohol flushing 10BV；The eluent rich in ginsenoside Rg1 is collected, is evaporated to obtain ginsenoside Rg1's crude product；
The proportioning of ginsenoside Rg1's crude product n-Butanol soluble, ginsenoside crude product (g) and n-butanol (mL) is 1：30, then use etc.
Volume aqueous phase extracts 4 times, collects n-butanol phase, is evaporated to obtain ginsenoside Rg1 0.92g；The purity of ginsenoside Rg1 is
99.2%.
Embodiment 4
Arasaponin 5.0g is dissolved in the ethanol of 25ml 95%；The neutral alumina aluminium powder of 300-400 mesh is weighed,
Post, column volume 250ml are filled after being soaked with 95% ethanol；By the ethanol solution loading of arasaponin, with 95% alcohol flushing
6BV, then with 85% alcohol flushing 12BV；The eluent rich in ginsenoside Rg1 is collected, is evaporated to obtain ginsenoside Rg1's crude product；
The proportioning of ginsenoside Rg1's crude product n-Butanol soluble, ginsenoside crude product (g) and n-butanol (mL) is 1：20, then use etc.
Volume aqueous phase extracts 4 times, collects n-butanol phase, is evaporated to obtain ginsenoside Rg1 0.95g；The purity of ginsenoside Rg1 is
98.7%.
Claims (9)
1. a kind of purification process of ginsenoside Rg1, it is characterised in that step is as follows：
(1) arasaponin is dissolved in 95% ethanol, obtains solution；
(2) neutral alumina aluminium powder is weighed, post is filled after being soaked with 95% ethanol；
(3) by step (1) obtained by solution loading；
(4) with 95% alcohol flushing, then with 85% alcohol flushing；
(5) eluent rich in ginsenoside Rg1 is collected, is evaporated to obtain ginsenoside Rg1's crude product；
(6) by ginsenoside Rg1's dissolving crude product obtained by step (5) in n-butanol phase, then extracted, received with isometric aqueous phase
Collect n-butanol phase, be evaporated to obtain ginsenoside Rg1.
2. the purification process of ginsenoside Rg1 according to claim 1, it is characterised in that arasaponin in step (1)
Proportioning with 95% ethanol is 1：5-1：10, arasaponin is in terms of g, and 95% ethanol is in terms of mL.
3. the purification process of ginsenoside Rg1 according to claim 1, it is characterised in that neutral alumina in step (2)
The mesh number of powder is 80-400 mesh.
4. the purification process of ginsenoside Rg1 according to claim 1, it is characterised in that neutral alumina in step (2)
The proportioning of powder and 95% ethanol is 1：2-1：5, neutral alumina aluminium powder is in terms of g, and 95% ethanol is in terms of mL.
5. the purification process of ginsenoside Rg1 according to claim 1, it is characterised in that arasaponin in step (2)
Quality and column volume ratio be 1：50, quality is in terms of g, and column volume is in terms of ml.
6. the purification process of ginsenoside Rg1 according to claim 1, it is characterised in that 95% ethanol rushes in step (4)
The flow washed is 4-6BV.
7. the purification process of ginsenoside Rg1 according to claim 1, it is characterised in that 85% ethanol rushes in step (4)
The flow washed is 10-12BV.
8. the purification process of ginsenoside Rg1 according to claim 1, it is characterised in that ginsenoside Rg1 in step (6)
The proportioning of crude product and n-butanol phase is 1：15-1：30, ginsenoside Rg1's crude product is in terms of g, and n-butanol is mutually in terms of mL.
9. the purification process of ginsenoside Rg1 according to claim 1, it is characterised in that extraction times are 4 in step (6)
It is secondary.
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| CN201711034686.6A CN107722100B (en) | 2017-10-30 | 2017-10-30 | Method for purifying ginsenoside Rg1 |
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| CN201711034686.6A CN107722100B (en) | 2017-10-30 | 2017-10-30 | Method for purifying ginsenoside Rg1 |
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| CN107722100A true CN107722100A (en) | 2018-02-23 |
| CN107722100B CN107722100B (en) | 2021-05-14 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005120536A1 (en) * | 2004-06-11 | 2005-12-22 | Unigen, Inc. | Ginseng composition for preventing or improving the lowering of concentration and memory capability |
| CN1869052A (en) * | 2006-06-21 | 2006-11-29 | 海南亚洲制药有限公司 | Method of extracting and separating ginseng saponine mixture from ginseng leaf |
| CN1869054A (en) * | 2006-06-21 | 2006-11-29 | 海南亚洲制药有限公司 | Preparation method of ginseng group saponine |
| CN105601693A (en) * | 2015-10-22 | 2016-05-25 | 大连大学 | Preparation method and antitumor effect of ginsenoside F1 |
-
2017
- 2017-10-30 CN CN201711034686.6A patent/CN107722100B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005120536A1 (en) * | 2004-06-11 | 2005-12-22 | Unigen, Inc. | Ginseng composition for preventing or improving the lowering of concentration and memory capability |
| CN1869052A (en) * | 2006-06-21 | 2006-11-29 | 海南亚洲制药有限公司 | Method of extracting and separating ginseng saponine mixture from ginseng leaf |
| CN1869054A (en) * | 2006-06-21 | 2006-11-29 | 海南亚洲制药有限公司 | Preparation method of ginseng group saponine |
| CN105601693A (en) * | 2015-10-22 | 2016-05-25 | 大连大学 | Preparation method and antitumor effect of ginsenoside F1 |
Non-Patent Citations (1)
| Title |
|---|
| 刘倩等: ""HPLC 检测人参皂苷在温和酸性条件下的降解产物"", 《大连医科大学学报》 * |
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| CN107722100B (en) | 2021-05-14 |
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Address after: 256100 No. 1 Yang drive road, Yiyuan County, Zibo, Shandong Applicant after: Ruiyang Pharmaceutical Co., Ltd Address before: 256100 No. 1 Yang drive road, Yiyuan County, Zibo, Shandong Applicant before: REYOUNG PHARMACEUTICAL Co.,Ltd. |
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