CN108992572A - A kind of extraction separation method of the non-polysaccharide component of rhizoma polygonati and application - Google Patents
A kind of extraction separation method of the non-polysaccharide component of rhizoma polygonati and application Download PDFInfo
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Abstract
The invention discloses a kind of extraction separation methods of the non-polysaccharide component of rhizoma polygonati, steps are as follows: dry rhizoma polygonati stem tuber is sliced, the ethyl alcohol of concentration 95% is added, carry out first time refluxing extraction, the ethyl alcohol of concentration 80% is added in the filter residue being obtained by filtration for the first time, carries out second of refluxing extraction, filtering, merge the filtrate extracted twice, is concentrated to get rhizoma polygonati coarse extract；Rhizoma polygonati coarse extract is added into distillation water dispersion, then successively with petroleum ether, n-butanol, ethyl acetate and methylene chloride extraction, respectively obtain petroleum ether phase, n-butanol phase, ethyl acetate phase, methylene chloride phase, methylene chloride phase and ethyl acetate phase are merged to obtain dichloromethane/ethyl acetate phase, organic solvent therein is recycled, the concentrated extract of 3 kinds of organic phases, drying at 60 DEG C are obtained, up to the non-polysaccharide component of rhizoma polygonati, dichloromethane/ethyl acetate phase antitumous effect is best.
Description
Technical field
The invention belongs to rhizoma polygonati extracting method technical fields, and in particular to a kind of extraction separation side of the non-polysaccharide component of rhizoma polygonati
Method and application.
Background technique
Rhizoma polygonati (Polygonatum sibiricum), also known as: polygonatum sibiricum Redoute, yellow chicken dish, pen tube dish, claw ginseng, tiger
Ginger, achickenclaw ginseng.For HUANGJING ZANYU CAPSULE, rhizome it is horizontal walk, cylindric, tubercle expands, impeller generator, stockless.Rhizoma polygonati nature and flavor are sweet, eat
It is tasty and refreshing, it is the integration of drinking and medicinal herbs Chinese herbal medicine of Chinese tradition, meat rhizomes is plump, contains much starch, sugar, fat, egg
White matter, carrotene, vitamin and various other nutritional ingredients, eat raw, stewing can allay one's hunger and body-building is used, and can make us gas
Power multiplication, muscle is full, marrow is strong, highly beneficial to body.Rhizoma polygonati main component Siberian solomonseal rhizome polysaccharide medical value is high, has
Antitumor, anti-oxidant, immunological regulation, antibacterial anti-inflammatory, hypoglycemic isoreactivity.The content of Siberian solomonseal rhizome polysaccharide is identification rhizoma polygonati quality
One highly important index.In health food, therapeutic pharmaceuticals, the great potential of the application of everyday skincare etc.
There is very vast market prospect；But Chinese Pharmacopoeia only has Siberian solomonseal rhizome polysaccharide content one to the quality control index of rhizoma polygonati at present
A index, characteristic component is indefinite, inadequate system, cannot identify rhizoma polygonati quality comprehensively, illustrate its material base.At present to rhizoma polygonati
The extracting method of active constituent has very much, mainly uses the alcohol precipitation method.
It is described as disclosed Rhizoma Polygonati extract and the preparation method and application thereof in number of patent application CN201410306492.7
Rhizoma Polygonati extract is prepared by the following method to obtain: after rhizoma polygonati ethyl alcohol heat mentions, extracting solution reduced-pressure backflow being obtained total medicinal extract；Add
Distilled water is suspended, and successively with isometric petroleum ether, ethyl acetate, extracting n-butyl alcohol, solvent is recovered under reduced pressure, and obtains ethyl acetate extraction
Position；The Rhizoma Polygonati extract has AGEs inhibiting effect, can further be applied to anti-diabetic and its complication medicine
Preparation, have important clinical value.Rhizoma polygonati is repeatedly extracted with ethyl alcohol in this application, and the concentration of ethyl alcohol is added all every time
Constant, and the addition sequence of extractant is petroleum ether, ethyl acetate and n-butanol in extraction process, extractant polarity by
It is small to arrive greatly, the effective component extraction rate in rhizoma polygonati can be made lower using this extracting method, and separate between each ingredient not thorough
Bottom, especially polysaccharide component and non-polysaccharide component, limit the application of rhizoma polygonati.
Summary of the invention
The purpose of the present invention is overcome the deficiencies of the prior art and provide a kind of extraction separation method of non-polysaccharide component of rhizoma polygonati
And application.
The present invention provides a kind of extraction separation methods of the non-polysaccharide component of rhizoma polygonati, which is characterized in that steps are as follows:
1) dry rhizoma polygonati stem tuber is sliced, the ethanol water of volumetric concentration 95% is added, carried out reflux for the first time and mention
It takes, the ethanol water of volumetric concentration 80% is added in the filter residue being obtained by filtration for the first time, carry out second of refluxing extraction, mistake
Filter merges the filtrate extracted twice, is concentrated to get rhizoma polygonati coarse extract；
2) rhizoma polygonati coarse extract is added into distillation water dispersion, then successively uses petroleum ether, n-butanol, ethyl acetate and methylene chloride
Extraction, respectively obtains petroleum ether phase, n-butanol phase, ethyl acetate phase, methylene chloride phase, by methylene chloride phase and ethyl acetate phase
Merging obtains dichloromethane/ethyl acetate phase, recycles to organic solvent therein, obtains the concentrated extract of 3 kinds of organic phases,
It dries at 60 DEG C to get the non-polysaccharide component of rhizoma polygonati.
Preferably, the ethanol water and rhizoma polygonati stem tuber that volumetric concentration 95% is added are extracted in the step 1) for the first time
Mass ratio is 5-6:1.
Preferably, the time of first time refluxing extraction is 2-3h in the step 1).
Preferably, second of ethanol water for extracting addition volumetric concentration 80% and first time filter in the step 1)
Filter residue mass ratio be 4-5:1.
Preferably, the time of second of refluxing extraction is 1-2h in the step 1).
Preferably, the condition being concentrated in the step 1) are as follows: temperature is 50-60 DEG C, and vacuum degree is -0.09MPa, concentrate
Specific gravity is 1-1.1.
Preferably, the temperature of refluxing extraction is 80-90 DEG C twice in the step 1).
The present invention also provides the non-polysaccharide components of rhizoma polygonati obtained according to said extracted separation method in anti-tumor aspect
Using.
3 kinds of organic phases obtained in step 2) of the present invention, i.e. petroleum ether phase, n-butanol phase, ethyl acetate/dichloromethane
Alkane phase recycles organic solvent therein, and 60 DEG C of dryings of concentrate can be used for preparing antitumor medicine or health care product.
Being usually used in the extracting method of rhizoma polygonati active constituent at present is that alcohol extracting is followed the example of, and is readily dissolved in using rhizoma polygonati active constituent
In ethyl alcohol, extracted.Rhizoma polygonati is repeatedly extracted with ethyl alcohol, and the concentration of addition ethyl alcohol is all constant every time, and what is obtained mentions
Take liquid that extractant extraction is added, the addition sequence of extractant is according to the ascending (number of patent application of polarity
CN201410306492.7), can make the effective component extraction rate in rhizoma polygonati lower using this extracting method, and respectively at point it
Between separate and be not thorough, especially polysaccharide component and non-polysaccharide component limit the application of rhizoma polygonati.
Rhizoma polygonati stem tuber is used the ethanol water of volumetric concentration 95% and the ethanol water of volumetric concentration 80% by the present invention respectively
Solution circulation carries out refluxing extraction twice, through research, the inventor has found that, the concentration of the control ethyl alcohol of refluxing extraction addition twice
It is different, and it is respectively 95% and 80% that the volumetric concentration of ethyl alcohol is only added twice, it can be to the greatest extent by rhizoma polygonati
In non-polysaccharide component extract, realize the effective use of rhizoma polygonati.In addition, extraction is added by obtained extracting solution is extracted in the present invention
It takes agent to be extracted, is firstly added petroleum ether and ungrease treatment is carried out to rhizoma polygonati ingredient, then successively use n-butanol, ethyl acetate again
It is further extracted with methylene chloride, obtains four organic phases and water phase；The addition that the present invention has broken current conventional extraction agent is suitable
Sequence (i.e. ascending by polarity), addition sequence of the discovery according to extractant of the present invention, the concentration of ethyl alcohol when in conjunction with refluxing extraction,
Effective component in rhizoma polygonati can adequately be separated, especially be non-polysaccharide component, realize rhizoma polygonati in terms of a variety of drugs
It efficiently utilizes, expands its application range.
Petroleum ether phase, n-butanol phase, ethyl acetate/dichloromethane phase and the water phase that the present invention is finally obtained by extraction carry out
Antitumor research finds that the antitumous effect of ethyl acetate/dichloromethane phase is best.
By ethyl acetate/dichloromethane mutually respectively by column chromatography, preparative high performance liquid chromatography and glucose repeatedly
Gel chromatography is isolated and purified, and 10 compounds, including 4 flavones, 2 alkaloids, 1 steroidal soap are finally separating to obtain
Glycosides, 1 daucosterol and 2 fatty acid.
The beneficial effects of the present invention are:
1, rhizoma polygonati stem tuber is used the ethanol water of volumetric concentration 95% and the ethyl alcohol of volumetric concentration 80% by the present invention respectively
Water solution cycle carries out refluxing extraction twice, through research, the inventor has found that, the dense of ethyl alcohol is added in refluxing extraction twice for control
Spend different, and it is respectively 95% and 80% that the concentration of ethyl alcohol is only added twice, can to the greatest extent will be in rhizoma polygonati
Non- polysaccharide component extract, realize the effective use of rhizoma polygonati.
2, the present invention has broken the addition sequence (i.e. ascending by polarity) of current conventional extraction agent, finds according to this hair
The addition sequence of bright extractant, the concentration of ethyl alcohol when in conjunction with refluxing extraction can adequately separate the effective component in rhizoma polygonati,
Especially polysaccharide component and non-polysaccharide component realize efficient utilization of the rhizoma polygonati in terms of a variety of drugs, expand it using model
It encloses.
3, preparation method of the present invention is simple, easy to operate, and the yield of the non-polysaccharide component of rhizoma polygonati is high, takes full advantage of rhizoma polygonati money
Source improves the use value of raw material, and this technology has no effect on the extraction of polysaccharide while extracting non-polysaccharide, returns
High income, low pollution (all organic solvents can recycle again).
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, to this hair
Bright further description.
Embodiment 1
1) dry rhizoma polygonati stem tuber is sliced, the ethanol water of volumetric concentration 95%, ethanol water and rhizoma polygonati is added
The mass ratio of stem tuber is 5:1, and first time refluxing extraction is carried out at 80 DEG C, after 2h, is added in the filter residue that is obtained by filtration for the first time
The mass ratio of the ethanol water of volumetric concentration 80%, 80% ethanol water and the filter residue filtered for the first time is 5:1,80
Second of refluxing extraction is carried out at DEG C, is filtered after 1h, is merged the filtrate extracted twice, is concentrated to get rhizoma polygonati coarse extract, concentration
Condition are as follows: temperature is 50 DEG C, and vacuum degree is -0.09MPa, and concentrate specific gravity is 1；
2) rhizoma polygonati coarse extract is added to the distillation water dispersion of 2 times of quality, then successively uses petroleum ether, n-butanol, ethyl acetate
It is extracted with methylene chloride, obtains petroleum ether phase, n-butanol phase, ethyl acetate phase, methylene chloride phase and water phase after the completion of extraction, it will
Methylene chloride phase and ethyl acetate phase merge to obtain dichloromethane/ethyl acetate phase, and the non-polysaccharide component in final rhizoma polygonati is mentioned
It gets in 3 kinds of organic phases, i.e. petroleum ether phase, n-butanol phase, ethyl acetate/dichloromethane phase, organic solvent therein is carried out
Recycling, obtains the concentrated extract of 3 kinds of organic phases, and concentrated extract is dried at 60 DEG C to get the non-polysaccharide component of rhizoma polygonati, final rhizoma polygonati
The recovery rate of non-polysaccharide is 90.54%.
Embodiment 2
1) dry rhizoma polygonati stem tuber is sliced, the ethanol water of volumetric concentration 95%, 95% ethanol water is added
It is 6:1 with the mass ratio of rhizoma polygonati stem tuber, carries out first time refluxing extraction at 88 DEG C, after 3h, the filter residue that is obtained by filtration for the first time
The mass ratio of the middle ethanol water that volumetric concentration 80% is added, 80% ethanol water and the filter residue filtered for the first time is 5:
1, second of refluxing extraction is carried out at 88 DEG C, is filtered after 2h, is merged the filtrate extracted twice, is concentrated to get rhizoma polygonati coarse extract,
The condition of concentration are as follows: temperature is 55 DEG C, and vacuum degree is -0.09MPa, and concentrate specific gravity is 1.06；
2) rhizoma polygonati coarse extract is added to the distillation water dispersion of 2 times of quality, then successively uses petroleum ether, n-butanol, ethyl acetate
It is extracted with methylene chloride, obtains petroleum ether phase, n-butanol phase, ethyl acetate phase, methylene chloride phase and water phase after the completion of extraction, it will
Methylene chloride phase and ethyl acetate phase merge to obtain dichloromethane/ethyl acetate phase, and the non-polysaccharide component in final rhizoma polygonati is mentioned
It gets in 3 kinds of organic phases, i.e. petroleum ether phase, n-butanol phase, ethyl acetate/dichloromethane phase, organic solvent therein is carried out
Recycling, obtains the concentrated extract of 3 kinds of organic phases, and concentrated extract is dried at 60 DEG C to get the non-polysaccharide component of rhizoma polygonati, final rhizoma polygonati
The recovery rate of non-polysaccharide is 93.68%.
Embodiment 3
1) dry rhizoma polygonati stem tuber is sliced, the ethanol water of volumetric concentration 95%, ethanol water and rhizoma polygonati is added
The mass ratio of stem tuber is 5.5:1, and first time refluxing extraction is carried out at 90 DEG C, after 2.5h, in the filter residue that is obtained by filtration for the first time
The ethanol water of volumetric concentration 80% is added, 80% ethanol water and for the first time mass ratio of the filter residue of filtering are 4:1,
Second of refluxing extraction is carried out at 90 DEG C, is filtered after 1.5h, is merged the filtrate extracted twice, is concentrated to get rhizoma polygonati coarse extract,
The condition of concentration are as follows: temperature is 60 DEG C, and vacuum degree is -0.09MPa, and concentrate specific gravity is 1.1；
2) rhizoma polygonati coarse extract is added to the distillation water dispersion of 2 times of quality, then successively uses petroleum ether, n-butanol, ethyl acetate
It is extracted with methylene chloride, obtains petroleum ether phase, n-butanol phase, ethyl acetate phase, methylene chloride phase and water phase after the completion of extraction, it will
Methylene chloride phase and ethyl acetate phase merge to obtain dichloromethane/ethyl acetate phase, and the non-polysaccharide component in final rhizoma polygonati is mentioned
It gets in 3 kinds of organic phases, i.e. petroleum ether phase, n-butanol phase, ethyl acetate/dichloromethane phase, organic solvent therein is carried out
Recycling, obtains the concentrated extract of 3 kinds of organic phases, and concentrated extract is dried at 60 DEG C to get the non-polysaccharide component of rhizoma polygonati, final rhizoma polygonati
The recovery rate of non-polysaccharide is 91.22%.
Comparative example 1
1) dry rhizoma polygonati stem tuber is sliced, the ethanol water of volumetric concentration 80%, 80% ethanol water is added
It is 6:1 with the mass ratio of rhizoma polygonati stem tuber, carries out first time refluxing extraction at 88 DEG C, after 3h, the filter residue that is obtained by filtration for the first time
The mass ratio of the middle ethanol water that volumetric concentration 80% is added, 80% ethanol water and the filter residue filtered for the first time is 5:
1, second of refluxing extraction is carried out at 88 DEG C, is filtered after 2h, is merged the filtrate extracted twice, is concentrated to get rhizoma polygonati coarse extract,
The condition of concentration are as follows: temperature is 55 DEG C, and vacuum degree is -0.09MPa, and concentrate specific gravity is 1.06；
2) rhizoma polygonati coarse extract is added to the distillation water dispersion of 2 times of quality, then successively uses petroleum ether, n-butanol, ethyl acetate
It is extracted with methylene chloride, obtains petroleum ether phase, n-butanol phase, ethyl acetate phase, methylene chloride phase and water phase after the completion of extraction, it will
Methylene chloride phase and ethyl acetate phase merge to obtain dichloromethane/ethyl acetate phase, and the non-polysaccharide component in final rhizoma polygonati is mentioned
It gets in 3 kinds of organic phases, i.e. petroleum ether phase, n-butanol phase, ethyl acetate/dichloromethane phase, organic solvent therein is carried out
Recycling, obtains the concentrated extract of 3 kinds of organic phases, and concentrated extract is dried at 60 DEG C to get the non-polysaccharide component of rhizoma polygonati, final rhizoma polygonati
The recovery rate of non-polysaccharide is 78.31%.
Comparative example 2
1) dry rhizoma polygonati stem tuber is sliced, the ethanol water of volumetric concentration 95%, 95% ethanol water is added
It is 6:1 with the mass ratio of rhizoma polygonati stem tuber, carries out first time refluxing extraction at 88 DEG C, after 3h, the filter residue that is obtained by filtration for the first time
The mass ratio of the middle ethanol water that volumetric concentration 80% is added, 80% ethanol water and the filter residue filtered for the first time is 5:
1, second of refluxing extraction is carried out at 88 DEG C, is filtered after 2h, is merged the filtrate extracted twice, is concentrated to get rhizoma polygonati coarse extract,
The condition of concentration are as follows: temperature is 55 DEG C, and vacuum degree is -0.09MPa, and concentrate specific gravity is 1.06；
2) rhizoma polygonati coarse extract is added to the distillation water dispersion of 2 times of quality, then successively uses petroleum ether, n-butanol, ethyl acetate
It is extracted with methylene chloride, obtains petroleum ether phase, methylene chloride phase, ethyl acetate phase, n-butanol phase and water phase after the completion of extraction, it will
Methylene chloride phase and ethyl acetate phase merge to obtain dichloromethane/ethyl acetate phase, and the non-polysaccharide component in final rhizoma polygonati is mentioned
It gets in 3 kinds of organic phases, i.e. petroleum ether phase, ethyl acetate/dichloromethane phase, n-butanol phase, organic solvent therein is carried out
Recycling, obtains the concentrated extract of 3 kinds of organic phases, and concentrated extract is dried at 60 DEG C to get the non-polysaccharide component of rhizoma polygonati, final rhizoma polygonati
The recovery rate of non-polysaccharide is 85.41%.
The recovery rate of the non-polysaccharide of rhizoma polygonati has reached 90% or more in 1-3 of the embodiment of the present invention, is higher than comparative example 1-2, says
It is bright using extracting method of the invention, the non-polysaccharide component in rhizoma polygonati can be sufficiently separated out, realize rhizoma polygonati a variety of
Efficient utilization in terms of drug, expands its application range.
The antitumor activity of each extraction phase of rhizoma polygonati
1, anticancer experiment in vitro
By petroleum ether phase, dichloromethane/ethyl acetate phase obtained in embodiment 2, n-butanol phase and water phase, recycling examination
Agent, respectively 60 DEG C of dryings, drying sample carry out anticancer experiment in vitro.
1.1 building cell culture and relevant cell library platform
Table 1 tests cell line used
1.2 experimental section
1.2.1MTT method analyzes influence of the different extraction phases to tumor cell proliferation
Experimental principle: there are succinate dehydrogenase on the mitochondrial inner membrane of living cells, which can be by the thiazolyl blue of yellow green
(referred to as MTT receives hydrionic dyestuff to be a kind of) is degraded into bluish violet formazan, and living cells is more, the bluish violet of generation
Formazan is more, and dead cell because on its mitochondrial inner membrane succinate dehydrogenase activity disappear, without this function.Use diformazan
Base sulfoxide dissolves the formazan of bluish violet, and absorbance value is measured at 490nm wavelength with microplate reader, can be gone out with quantitative reaction living thin
Born of the same parents' quantity.
1.2.2 different extraction phases inhibit HepG-2 and MCF-7 cell proliferation experiment
(1) experimental group: experiment is divided into water phase, n-butanol phase, dichloromethane/ethyl acetate phase, petroleum ether phase and control
Group.Using cyclophosphamide as positive controls；It is all provided with 3 multiple holes for every group above.
(2) cell culture: original fluid, sterile PBS washing is sucked out in HepG-2 the and MCF-7 cell of logarithmic growth phase
Suitable pancreatin is added afterwards twice to be digested, and cell is collected by centrifugation, cell suspension is made；Cell is counted, and dilute
Releasing cell concentration is 7x104/ ml prepares 96 sterile porocyte culture plates and is marked accordingly, and then every hole is added 100
μ l cell suspension, sets 37 DEG C, 5%CO2Culture in incubator.When cell adherent growth is to 80% or so, the every hole of experimental group adds
Enter corresponding drug, sets 37 DEG C, 5%CO248h is cultivated in incubator.Original fluid is sucked out, sterile PBS washes twice rear every hole
The culture medium that the MTT containing 0.5mg/mL is added continues to cultivate 4h.Culture medium in hole is carefully sucked out after 4h, 150 μ l diformazans are added in every hole
Base sulfoxide, sets and at the uniform velocity shakes 10min on shaking table, makes to crystallize abundant dissolution.Each group extinction is measured at 490nm wavelength with microplate reader again
Angle value calculates cell proliferation inhibition rate.
1.3 results and analysis
1.3.1MTT laboratory test results
After acting on HepG-2 and MCF-7 cell for 24 hours with different extraction phases, microplate reader measures each hole absorbance, and
Cell proliferation inhibition rate is calculated, the results are shown in Table 2, wherein IC50 is rate half-suppressed.
Inhibiting effect of the different extraction phases of table 2 to tumor cell line
From the data in table 2 it is found that different extraction phases of the invention all have breast cancer and liver cancer kinds of tumor cells
Stronger inhibiting effect shows extraordinary antitumor efficacy, and wherein the antitumous effect of dichloromethane/ethyl acetate phase is most
It is good, it is better than water phase, achieves unexpected technical effect.
2, internal anti-tumor experiment
By petroleum ether phase, dichloromethane/ethyl acetate phase obtained in embodiment 2, n-butanol phase and water phase, recycling examination
Agent, respectively 60 DEG C of dryings, drying sample carry out internal anti-tumor experiment respectively.
2.1 experimental raw
Experiment is divided into water phase, n-butanol phase, dichloromethane/ethyl acetate phase, petroleum ether phase and control group, with cyclophosphamide
For positive controls.
2.2 experimental method
Experimental animal: Kunming mouse, 18~22g of weight, male and female dual-purpose are taken.The lung cancer Lewis tumor mass of inoculation 10 days is taken,
Lewis cell suspension (cell number 1 × 10 is made7/ ml), in addition to healthy control group, remaining mouse upper limb right axillary inoculates lung
Cancer Lewis cell suspension 0.2ml is randomly divided into after inoculation 24 hours as physiological saline group 20ml/kg, petroleum ether phase, dichloromethane
The drying sample experimental group 3g/kg of alkane/ethyl acetate phase, n-butanol phase and water phase respectively, cyclophosphamide (CTX) control group
60mg/kg intraperitoneal injection.The equal successive administration of each group 14 days takes tumor mass to weigh, calculates tumor suppression with the whole mouse of execution in the 15th day
Rate.The results are shown in Table 3 for specific experiment.
Inhibiting effect of the different extraction phases of table 3 to mice lung cancer Lewis
Note: compared with physiological saline group, P < 0.05 *；**P<0.01.
By data antitumor in 3 body of table it is found that petroleum ether phase, dichloromethane/ethyl acetate phase, just that the present invention obtains
Butanol phase and water phase can effectively inhibit the growth of Mice Bearing Lewis Lung Cancer, and wherein dichloromethane/ethyl acetate phase is antitumor
Effect is best, is better than water phase, achieves unexpected technical effect.
Claims (8)
1. a kind of extraction separation method of the non-polysaccharide component of rhizoma polygonati, which is characterized in that steps are as follows:
1) dry rhizoma polygonati stem tuber is sliced, the ethanol water of volumetric concentration 95% is added, carry out first time refluxing extraction, the
The ethanol water of volumetric concentration 80% is added in the filter residue being once obtained by filtration, carries out second of refluxing extraction, filters, merges
The filtrate extracted twice is concentrated to get rhizoma polygonati coarse extract；
2) rhizoma polygonati coarse extract is added into distillation water dispersion, then successively with petroleum ether, n-butanol, ethyl acetate and methylene chloride extraction
It takes, respectively obtains petroleum ether phase, n-butanol phase, ethyl acetate phase, methylene chloride phase, methylene chloride phase and ethyl acetate are harmonious
And dichloromethane/ethyl acetate phase is obtained, and organic solvent therein is recycled, obtains the concentrated extract of 3 kinds of organic phases, 60
It dries at DEG C to get the non-polysaccharide component of rhizoma polygonati.
2. the extraction separation method of the non-polysaccharide component of rhizoma polygonati as described in claim 1, which is characterized in that in the step 1)
The primary mass ratio for extracting ethanol water and rhizoma polygonati stem tuber that volumetric concentration 95% is added is 5-6:1.
3. the extraction separation method of the non-polysaccharide component of rhizoma polygonati as described in claim 1, which is characterized in that in the step 1)
The time of refluxing extraction is 2-3h.
4. the extraction separation method of the non-polysaccharide component of rhizoma polygonati as described in claim 1, which is characterized in that in the step 1)
The ethanol water of volumetric concentration 80% is added for second extraction and the mass ratio of the filter residue of filtering is 4-5:1 for the first time.
5. the extraction separation method of the non-polysaccharide component of rhizoma polygonati as claimed in claim 1 or 2, which is characterized in that the step 1)
In second of refluxing extraction time be 1-2h.
6. the extraction separation method of the non-polysaccharide component of rhizoma polygonati as claimed in claim 1 or 2, which is characterized in that the step 1)
The condition of middle concentration are as follows: temperature is 50-60 DEG C, and vacuum degree is -0.09MPa, and concentrate specific gravity is 1-1.1.
7. the extraction separation method of the non-polysaccharide component of rhizoma polygonati as claimed in claim 1 or 2, which is characterized in that the step 1)
In twice refluxing extraction temperature be 80-90 DEG C.
8. application of the non-polysaccharide component of rhizoma polygonati in anti-tumor aspect as described in claim any one of 1-3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811010905.1A CN108992572B (en) | 2018-08-31 | 2018-08-31 | Extraction and separation method and application of non-polysaccharide components of polygonatum sibiricum |
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| WO2006099804A1 (en) * | 2005-03-23 | 2006-09-28 | Lee's Pharmaceutical (Hong Kong) Limited | Herbal compositions useful in cancer treatment |
| CN104069348A (en) * | 2014-06-30 | 2014-10-01 | 天津中医药大学 | Sealwort extract as well as preparation method and use thereof |
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| WO2006099804A1 (en) * | 2005-03-23 | 2006-09-28 | Lee's Pharmaceutical (Hong Kong) Limited | Herbal compositions useful in cancer treatment |
| CN104069348A (en) * | 2014-06-30 | 2014-10-01 | 天津中医药大学 | Sealwort extract as well as preparation method and use thereof |
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