CN106432392A - Preparation method of ginsenoside Rg1 and ginsenoside Re - Google Patents
Preparation method of ginsenoside Rg1 and ginsenoside Re Download PDFInfo
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- CN106432392A CN106432392A CN201610792895.6A CN201610792895A CN106432392A CN 106432392 A CN106432392 A CN 106432392A CN 201610792895 A CN201610792895 A CN 201610792895A CN 106432392 A CN106432392 A CN 106432392A
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Abstract
The invention relates to a preparation method of ginsenoside Rg1 and ginsenoside Re, and belongs to the technical field of medicine. The preparation method comprises the steps that 1 g of total saponins of panax ginseng are taken to be dissolved into a 20% acetonitrile solution, the obtained mixture is taken as a sample, and gradient eluting is conducted through a preparative high performance liquid chromatograph, wherein SinoChrom ODS-BP with the specification of 200 mm*20 mm and 10 micrometers is taken as a chromatographic column, the detection wavelength is 203 nm, the flow speed is 15 ml/min, and the sample feeding amount is 5 ml; eluent of ginsenoside Rg1 and eluent of ginsenoside Re are collected separately, pressure reduction is conducted on the eluents at the low temperature of 50 DEG C or below for recycling acetonitrile, then vacuum concentration is conducted at the high temperature of 60 DEG C to 80 DEG C, vacuum freeze drying is conducted on concentrated liquid, and then freeze-dried powder is prepared. The preparation method has the advantages that the production cost is reduced, environmental friendliness is achieved, the production period is short, the purity of obtained ginsenoside monomers is 90% or above and reaches the purity of a reference substance for content determination, and the yield can reach 80% or above and is much higher than that of a traditional preparation method.
Description
Technical field
The invention belongs to field of medicaments, be specifically related to a kind of system simultaneously obtaining high-purity ginsenoside monomer Rg1 and Re
Preparation Method.
Background technology
Ginseng is famous and precious tonic herb, has and reinforces vital energy, and multiple arteries and veins takes off admittedly, reinforces the spleen to benefit the lung, promotes the production of body fluid and nourish blood, intelligence development of calming the nerves
Effect.Its active ingredient is mainly ginsenoside, and current isolated ginsenoside is more than 30 kinds.Ginsenoside Rg1 and
Re has it to cardiovascular system, immune system, neural protection and obvious antitumor action.Because of ginsenoside list
Body belongs to natural drug, has curative effect high, and the advantages such as toxic and side effect is little, development and application has a extensive future.
Prepared by present separation using Flavonoids by Macroporous Adsorption Resin to carry out ginsenoside monomer more, but, the method uses big
The organic solvents such as the chloroform of amount, acetone, methyl alcohol, n-butanol, and be difficult to reclaim, big for environment pollution, and the production cycle is long, substantially
In even several months several weeks, additionally, complex manufacturing, complex operation, mechanization, automaticity are low, it is difficult to realize industrialization
Big production, the ginsenoside monomer purity produced is low, and substantially below 90%, yield is not high, how below 60%.
Content of the invention
The present invention provides the preparation method of a kind of ginsenoside Rg_1 and Re, to solve the ginsenoside Rg1 producing at present
Low with Re monomer purity, the not high problem of yield.
The technical solution used in the present invention is, step is as follows：
Take general ginsenoside or ginseng stem and leave general saponin 1g is dissolved in 20% acetonitrile solution, as sample, use preparative high
Effect liquid phase chromatogram instrument, with SinoChrom ODS-BP 200mm × 20mm 10 μm as chromatographic column, detects wavelength 203nm, flow velocity
15ml/min, sample size 5ml；Carry out gradient elution by table 1,
Table 1 gradient elution table
Collecting ginsenoside Rg1, the eluent of Re respectively, eluent first low-temperature reduced-pressure below 50 DEG C reclaims acetonitrile, after
60-80 DEG C of high-temperature pressure-reduction concentrates, and concentrate vacuum freeze drying prepares freeze-dried powder.
Described ginseng stem and leave general saponin is：Take gen-seng haulms, be cut into 1-2cm section, add boiling water twice, 2 hours for the first time,
1.5 hours for the second time, decoction liquor filtered, merging filtrate, and by D101 type large pore resin absorption column, water elution is extremely colourless, then uses
60% ethanol elution, collects 60% ethanol eluate, surveys the clear cream that relative density is 1.06-1.08 when filtrate is concentrated into 80 DEG C,
Dry, pulverize, to obtain final product.
Described general ginsenoside is：Taking ginseng, being cut into sheet, add boiling water twice, 2 hours for the first time, 1.5 is little for the second time
When, decoction liquor filters, merging filtrate, and by D101 type large pore resin absorption column, water elution is extremely colourless, then is washed by 60% ethanol
De-, collect 60% ethanol eluate, survey the clear cream that relative density is 1.06-1.08 when filtrate is concentrated into 80 DEG C, dry, pulverize,
Obtain.
Advantages of the present invention is as follows：
1st, economy, environmental protection：Use acetonitrile and water as solvent, and acetonitrile had been carried out time before eluent vacuum freeze-drying
Receive, can be recycled after dehydration, greatly reduce production cost, both economically and environmentally beneficial.
2nd, production technology is simple, with short production cycle：Only need a preparative high performance liquid chromatography instrument just can realize people
Ginseng soap efficiently separating with Rg1 and Re, disengaging time within 50min, whole separation cycle within 100min, eluent warp
After recycling design, use a vacuum freeze drier, i.e. can get highly purified ginsenoside monomer.
3rd, yield is high, purity is big：The ginsenoside monomer purity obtaining, more than 90%, has reached assay comparison
The purity of product, yield can reach more than 80%, far above traditional preparation method.
Detailed description of the invention
General ginsenoside used by the present invention or ginseng stem and leave general saponin can be obtained by purchase, or make as follows
Standby：
Ginseng stem and leave general saponin is prepared as：Take gen-seng haulms, be cut into 1-2cm section, add boiling water twice, 2 hours for the first time,
1.5 hours for the second time, decoction liquor filtered, merging filtrate, and by D101 type large pore resin absorption column, water elution is extremely colourless, then uses
60% ethanol elution, collects 60% ethanol eluate, surveys the clear cream that relative density is 1.06-1.08 when filtrate is concentrated into 80 DEG C,
Dry, pulverize, to obtain final product.
General ginsenoside is prepared as：Taking ginseng, being cut into sheet, add boiling water twice, 2 hours for the first time, 1.5 is little for the second time
When, decoction liquor filters, merging filtrate, and by D101 type large pore resin absorption column, water elution is extremely colourless, then is washed by 60% ethanol
De-, collect 60% ethanol eluate, survey the clear cream that relative density is 1.06-1.08 when filtrate is concentrated into 80 DEG C, dry, pulverize,
Obtain.
Embodiment 1
Take general ginsenoside 1g and be dissolved in 20% acetonitrile solution, as sample, use preparative high performance liquid chromatography instrument, with
SinoChrom ODS-BP 200mm × 20mm 10 μm is chromatographic column, detects wavelength 203nm, flow velocity 15ml/min, sample size
5ml；Carry out gradient elution by table 2,
Table 2 gradient elution table
Collecting ginsenoside Rg1, the eluent of Re respectively, eluent first reclaims acetonitriles at 50 DEG C of low-temperature reduced-pressures, latter 60 DEG C
High-temperature pressure-reduction concentrates, and concentrate vacuum freeze drying prepares freeze-dried powder.
Embodiment 2
Take general ginsenoside 1g and be dissolved in 20% acetonitrile solution, as sample, use preparative high performance liquid chromatography instrument, with
SinoChrom ODS-BP 200mm × 20mm 10 μm is chromatographic column, detects wavelength 203nm, flow velocity 15ml/min, sample size
5ml；Carry out gradient elution by table 3,
Table 3 gradient elution table
Collecting ginsenoside Rg1, the eluent of Re respectively, eluent first reclaims acetonitriles at 40 DEG C of low-temperature reduced-pressures, latter 70 DEG C
High-temperature pressure-reduction concentrates, and concentrate vacuum freeze drying prepares freeze-dried powder.
Embodiment 3
Take general ginsenoside 1g and be dissolved in 20% acetonitrile solution, as sample, use preparative high performance liquid chromatography instrument, with
SinoChrom ODS-BP 200mm × 20mm 10 μm is chromatographic column, detects wavelength 203nm, flow velocity 15ml/min, sample size
5ml；Carry out gradient elution by table 4,
Table 4 gradient elution table
Collecting ginsenoside Rg1, the eluent of Re respectively, eluent first low-temperature reduced-pressure below 25 DEG C reclaims acetonitrile, after
80 DEG C of high-temperature pressure-reductions concentrate, and concentrate vacuum freeze drying prepares freeze-dried powder.
Use method ibid each embodiment that ginseng stem and leave general saponin is prepared.
Claims (3)
1. the preparation method of a ginsenoside Rg_1 and Re, it is characterised in that step is as follows：Take general ginsenoside or gen-seng haulms
Total saposins 1g is dissolved in 20% acetonitrile solution, as sample, uses preparative high performance liquid chromatography instrument, with SinoChrom ODS-BP
200mm × 20mm 10 μm is chromatographic column, detects wavelength 203nm, flow velocity 15ml/min, sample size 5ml；Carry out gradient by table 1 to wash
It is de-,
Table 1 gradient elution table
Collecting ginsenoside Rg1, the eluent of Re respectively, eluent first low-temperature reduced-pressure below 50 DEG C reclaims acetonitrile, rear 60-80
DEG C high-temperature pressure-reduction concentrates, and concentrate vacuum freeze drying prepares freeze-dried powder.
2. the preparation method of a kind of ginsenoside Rg_1 and Re according to claim 1, it is characterised in that：Described ginseng stem
Leaf total saposins is：Take gen-seng haulms, be cut into 1-2cm section, add boiling water twice, 2 hours for the first time, 1.5 hours for the second time, decoct
Liquid filters, merging filtrate, and by D101 type large pore resin absorption column, water elution is extremely colourless, then uses 60% ethanol elution, collects
60% ethanol eluate, surveys the clear cream that relative density is 1.06-1.08, dry, pulverize, to obtain final product when filtrate is concentrated into 80 DEG C.
3. the preparation method of a kind of ginsenoside Rg_1 and Re according to claim 1, it is characterised in that：Described ginseng is total
Saponin(e is：Taking ginseng, being cut into sheet, add boiling water twice, 2 hours for the first time, 1.5 hours for the second time, decoction liquor filtered, and merged
Filtrate, by D101 type large pore resin absorption column, water elution is extremely colourless, then uses 60% ethanol elution, collects 60% ethanol elution
Liquid, surveys the clear cream that relative density is 1.06-1.08, dry, pulverize, to obtain final product when filtrate is concentrated into 80 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610792895.6A CN106432392A (en) | 2016-08-31 | 2016-08-31 | Preparation method of ginsenoside Rg1 and ginsenoside Re |
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| CN201610792895.6A CN106432392A (en) | 2016-08-31 | 2016-08-31 | Preparation method of ginsenoside Rg1 and ginsenoside Re |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108619200A (en) * | 2018-07-11 | 2018-10-09 | 山西省芮城县红宝兽药有限责任公司 | General ginsenoside injection for animals |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102464693A (en) * | 2010-11-05 | 2012-05-23 | 李慧 | Ginsenoside Re extraction and separation method |
| CN104807905A (en) * | 2015-05-04 | 2015-07-29 | 中国人民解放军第三七一医院 | Method for determining contents of ginsenosides Rg1 and Re in Xinnaoning tablet |
| CN105801656A (en) * | 2014-12-30 | 2016-07-27 | 广西梧州制药（集团）股份有限公司 | Method for purifying Rg1, Re and Rb1 from Panax notoginsenosides |
-
2016
- 2016-08-31 CN CN201610792895.6A patent/CN106432392A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102464693A (en) * | 2010-11-05 | 2012-05-23 | 李慧 | Ginsenoside Re extraction and separation method |
| CN105801656A (en) * | 2014-12-30 | 2016-07-27 | 广西梧州制药（集团）股份有限公司 | Method for purifying Rg1, Re and Rb1 from Panax notoginsenosides |
| CN104807905A (en) * | 2015-05-04 | 2015-07-29 | 中国人民解放军第三七一医院 | Method for determining contents of ginsenosides Rg1 and Re in Xinnaoning tablet |
Non-Patent Citations (1)
| Title |
|---|
| 陈波等: "人参皂苷Re、Rg1标准对照品的高效液相色谱制备研究", 《实用预防医学》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108619200A (en) * | 2018-07-11 | 2018-10-09 | 山西省芮城县红宝兽药有限责任公司 | General ginsenoside injection for animals |
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