CN106905405A - A kind of method that aglycon is extracted from the root of Chinese clematis and application - Google Patents
A kind of method that aglycon is extracted from the root of Chinese clematis and application Download PDFInfo
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- CN106905405A CN106905405A CN201710139465.9A CN201710139465A CN106905405A CN 106905405 A CN106905405 A CN 106905405A CN 201710139465 A CN201710139465 A CN 201710139465A CN 106905405 A CN106905405 A CN 106905405A
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Abstract
The invention discloses a kind of method that aglycon is extracted from the root of Chinese clematis and application.The method is comprised the following steps：(1) it is powder to crush the root of Chinese clematis, crosses 65 mesh sieves, and total saponin extracts are obtained to ethanol, 1~2h of refluxing extraction, cold filtration is added in powder；(2) to hydrochloric acid solution is added in step (1) gained total saponin extracts, 0.5~2.5h is hydrolyzed in 60~100 DEG C, obtains hydrolyzate；(3) to petroleum ether is added in step (2) gained hydrolyzate, extract 2~3 times, separate petroleum ether layer and water layer, then to ethyl acetate is added in water layer, extract 2~3 times, concentrated in less than 60 DEG C；(4) dissolved to addition methyl alcohol in enriched product, then separated with preparation liquid phase, Fractional Collections efflux obtains aglycon.The inventive method is simple, is conducive to the hydrolysis of total saposins, is easy to extract aglycon.
Description
Technical field
The present invention relates to natural drug extractive technique field, and in particular to it is a kind of from the root of Chinese clematis extract aglycon method and
Using.
Background technology
The root of Chinese clematis is one of conventional Chinese medicine, with dispelling wind and eliminating dampness, the effect of removing obstruction in channels to relieve pain.《Chinese Pharmacopoeia》Version is received within 2015
The root of Chinese clematis of load is ranunculaceae plant root of Chinese clematis Clematis chinensis Osbeck., Clematis hexapetala Clematis
Hexapetala Pall.'s or northeast clematis Clematis manshurica Rupr. dries root and rhizome.
Root of Chinese clematis alias has radix smilacis sieboldi, cuneate lespedeza, windmill etc., and taste is pungent is salty, warm in nature, returns bladder warp, as in tradition
Medicine, China book on Chinese herbal medicine works described in its have wind-damp dispelling, degrading the channel, stopping numbness pain, disappear bone sticking the effects such as, be mainly used in treat wind
Arthritis with fixed pain caused by dampness bitterly, extremity numbness, muscle arteries and veins contraction, joint joint stuffiness, and all bone sticking swallow is the most frequently used of Chinese traditional treatment rheumatic Bi syndrome
Chinese medicine, and the multiple Chinese patent drugs with the root of Chinese clematis as raw material have also been listed by successfully research and development in succession, such as " Jingfukang capsule ".
The root of Chinese clematis and northeast clematis mainly contain saponin component, and Clematis hexapetala mainly contains flavones ingredient, and preceding
Difference of them is very big, while the root of Chinese clematis and the saponin(e contained by northeast clematis there is also difference, according to the literature and before us
Phase research finds that contain substantial amounts of triterpenoid saponin in the root of Chinese clematis and northeast clematis, its design feature is：1. aglycon is ivy
Sapogenin type and together a tartaric acid type；2. most of to have disaccharide chain, a sugar chain is connected to aglycon 28 in the way of ester bond；Separately
One sugar chain is connected in 3 of aglycon；Different asafoetide acyl group is often connected on 3.3 sugar chains, has considerable influence to the activity of aglycon.
Research shows, hederagenin have reduce the inflammatory signals such as NO, PGE2, TNF-α, IL-1 β and IL-6 because
The effect that sublist reaches, so as to suppress inflammatory signals conduction, reaches the suppression to inflammatory reaction and regulating and controlling effect；And oleanolic acid exists
Clinically it is usually used in treating infectious acute icteric hepatitis, glutamic-pyruvic transaminase and removing jaundice effect is reduced with obvious, improves
The symptom of viral and chronic persistant hepatitis patient, sign and liver function；Can be additionally used in psoriasis, rheumatic arthritis, kidney
Scorching oedema, cirrhotic ascites, acute, chronic hepatitis, stomachache stranguria with turbid discharge, metrorrhagia, traumatic injury, carbuncle swells, soreness and weakness of waist and knees, fetal irritability etc.
Disease.
Under normal circumstances, oleanolic acid and hederagenin exist with various plants with glycoside forms, and this is to both
Exploitation bring inconvenience.
The content of the invention
For above-mentioned deficiency of the prior art, the present invention provides a kind of method that aglycon is extracted from the root of Chinese clematis, purpose
It is to provide a kind of method for being easy to extract aglycon in the root of Chinese clematis.
To solve above-mentioned technical problem, the technical solution adopted by the present invention is：
A kind of method that aglycon is extracted from the root of Chinese clematis, comprises the following steps：
(1) root of Chinese clematis is crushed, crosses 60~80 mesh sieves, to 70%~95% ethanol is added in powder, returned in 30~50 DEG C
Stream extracts 1~2h, and cold filtration obtains total saponin extracts；Wherein, root of Chinese clematis powder quality and ethanol volume ratio are 1~3:40
~50；
(2) to the hydrochloric acid solution that concentration is 1~5mol/L is added in step (1) gained total saponin extracts, in 60~100
DEG C hydrolysis 0.5~2.5h, obtain hydrolyzate；Wherein, acid solution and total saponin extracts volume ratio are 1~5:1~3；
(3) it is by volume 1:1 ratio is extracted 2~3 times to petroleum ether is added in step (2) gained hydrolyzate, is separated
Petroleum ether layer and water layer, then be by volume 1~1.5:1~2 ratio is extracted 2~3 times to ethyl acetate is added in water layer,
Concentrated in less than 60 DEG C, enriched product is obtained.
(4) dissolved to addition methyl alcohol in enriched product, then separated with preparation liquid phase, mobile phase is water and methyl alcohol, is divided
Section collects efflux, obtains aglycon.
Further, ethanol mass concentration is 70% ethanol in step (1).
Further, root of Chinese clematis powder quality and ethanol volume ratio are 1 in step (1):50.
Further, acid solution is hydrochloric acid, sulfuric acid, oxalic acid or boric acid in step (2).
Further, hydrolysising condition is in step (2)：In 100 DEG C, concentration are for the acid solution of 2mol/L, 1h is hydrolyzed.
Further, acid solution and total saposins volume ratio are 1.2 in step (2):1.
Further, ethyl acetate and water layer volume ratio are 1 in step (3):1.
Further, liquid phase separation gradient is prepared in step (4) is：Mobile phase is water and methyl alcohol, and column temperature is room temperature, 0~
30min, 60%~90% methyl alcohol, 40%~10% water；Flow velocity 5mL/min.
The aglycon that the above method is prepared.
Application of the above-mentioned aglycon in medicine for treating rheumatoid arthritis preparation.
Beneficial effects of the present invention are：
Total saponin extracts produce a large amount of aglycons after hydrolysis, are easy to subsequently carry out extraction separation to aglycon.
Petroleum ether extraction can remove the lipid impurities in hydrolyzate, and then hydrolyzate is extracted using ethyl acetate again
Take, not only increase the extraction efficiency of ethyl acetate, also improve the DNA purity of aglycon, be conducive to extracting and collect high-purity
Aglycon.
Brief description of the drawings
Fig. 1 is the chromatograms of the total saponin extracts that the present invention is prepared.
Specific embodiment
Specific embodiment of the invention is described below, this hair is understood in order to those skilled in the art
It is bright, it should be apparent that the invention is not restricted to the scope of specific embodiment, for those skilled in the art,
As long as in appended claim restriction and the spirit and scope of the present invention for determining, these changes are aobvious and easy to various change
See, all are using the innovation and creation of present inventive concept in the row of protection.
Embodiment 1
A kind of method that aglycon is extracted from the root of Chinese clematis, comprises the following steps：
(1) it is powder to crush the root of Chinese clematis, crosses 65 mesh sieves, to 70% ethanol is added in powder, in 45 DEG C of refluxing extraction 1h,
Cold filtration, obtains total saponin extracts；Wherein, root of Chinese clematis powder quality and ethanol volume ratio are 1:50；
(2) it is the hydrochloric acid solution of 2mol/L to concentration is added in step (1) gained total saponin extracts, in 100 DEG C of hydrolysis
1h, obtains hydrolyzate；Wherein, acid solution and total saponin extracts volume ratio are 1.2:1；
(3) it is by volume 1:1 ratio is extracted 2 times to petroleum ether is added in step (2) gained hydrolyzate, separates stone
Oily ether layer and water layer, then be by volume 1:1 ratio is extracted 2 times to ethyl acetate is added in water layer, is carried out in less than 60 DEG C
Concentration；
(4) to adding methyl alcohol to dissolve in enriched product, 10mL is settled to, obtains extract solution.
Embodiment 2
A kind of method that aglycon is extracted from the root of Chinese clematis, comprises the following steps：
(1) it is powder to crush the root of Chinese clematis, crosses 60 mesh sieves, to 95% ethanol is added in powder, in 30 DEG C of refluxing extraction 2h,
Cold filtration, obtains total saponin extracts；Wherein, root of Chinese clematis powder quality and ethanol volume ratio are 3:40；
(2) it is the hydrochloric acid solution of 1mol/L to concentration is added in step (1) gained total saponin extracts, in 60 DEG C of hydrolysis
0.5h, obtains hydrolyzate；Wherein, acid solution and total saponin extracts volume ratio are 1:3；
(3) it is by volume 1:1 ratio is extracted 3 times to petroleum ether is added in step (2) gained hydrolyzate, separates stone
Oily ether layer and water layer, then be by volume 1:2 ratio is extracted 3 times to ethyl acetate is added in water layer, is carried out in less than 60 DEG C
Concentration；
(4) to adding methyl alcohol to dissolve in enriched product, 10mL is settled to, obtains extract solution.
Embodiment 3
A kind of method that aglycon is extracted from the root of Chinese clematis, comprises the following steps：
(1) it is powder to crush the root of Chinese clematis, crosses 80 mesh sieves, to 80% ethanol is added in powder, in 50 DEG C of refluxing extraction 2h,
Cold filtration, obtains total saponin extracts；Wherein, root of Chinese clematis powder quality and ethanol volume ratio are 1:40；
(2) it is the hydrochloric acid solution of 5mol/L to concentration is added in step (1) gained total saponin extracts, in 80 DEG C of hydrolysis
2.5h, obtains hydrolyzate；Wherein, acid solution and total saponin extracts volume ratio are 5:3；
(3) it is by volume 1:1 ratio is extracted 2 times to petroleum ether is added in step (2) gained hydrolyzate, separates stone
Oily ether layer and water layer, then be by volume 1.5:2 ratio is extracted 2 times to ethyl acetate is added in water layer, is entered in less than 60 DEG C
Row concentration；
(4) to adding methyl alcohol to dissolve in enriched product, 10mL is settled to, obtains extract solution.
Embodiment 4
A kind of method extracted from the root of Chinese clematis in aglycon, comprises the following steps：
(1) it is powder to crush the root of Chinese clematis, crosses 65 mesh sieves, to 70% ethanol is added in powder, in 50 DEG C of refluxing extraction 1h,
Cold filtration, obtains total saponin extracts；Wherein, root of Chinese clematis powder quality and ethanol volume ratio are 1:50；
(2) it is the hydrochloric acid solution of 3mol/L to concentration is added in step (1) gained total saponin extracts, in 70 DEG C of hydrolysis
1.5h, obtains hydrolyzate；Wherein, acid solution and total saponin extracts volume ratio are 1.2:1；
(3) it is by volume 1:1 ratio is extracted 2 times to petroleum ether is added in step (2) gained hydrolyzate, separates stone
Oily ether layer and water layer, then be by volume 1:1 ratio is extracted 2 times to ethyl acetate is added in water layer, is carried out in less than 60 DEG C
Concentration；
(4) to adding methyl alcohol to dissolve in enriched product, 10mL is settled to, obtains extract solution.
Embodiment 5
A kind of method that aglycon is extracted from the root of Chinese clematis, comprises the following steps：
(1) it is powder to crush the root of Chinese clematis, 65 mesh sieves is crossed, to 90% ethanol is added in powder, in 50 DEG C of refluxing extractions
1.5h, cold filtration obtains total saponin extracts；Wherein, root of Chinese clematis powder quality and ethanol volume ratio are 1:50；
(2) it is the hydrochloric acid solution of 4mol/L to concentration is added in step (1) gained total saponin extracts, in 90 DEG C of hydrolysis
2h, obtains hydrolyzate；Wherein, acid solution and total saponin extracts volume ratio are 4:1.5；
(3) it is by volume 1:1 ratio is extracted 3 times to petroleum ether is added in step (2) gained hydrolyzate, separates stone
Oily ether layer and water layer, then be by volume 1:1 ratio is extracted 2 times to ethyl acetate is added in water layer, is carried out in less than 60 DEG C
Concentration；
(4) to adding methyl alcohol to dissolve in enriched product, 10mL is settled to, obtains extract solution.
Embodiment 6
Detection separation is carried out with respect to the products therefrom of embodiment 1 using preparation solution, chromatographic column is YMC-PacK ODS-A
(250mm*20mm), testing conditions are shown in Table 1, and chromatogram is shown in Fig. 1.
The chromatographic test strip part of table 1
Efflux is collected respectively at 12.2min, 24.7min and 51.2min, is concentrated under reduced pressure, obtain the list of different time sections
Body compound, its composition is shown in Table 2.
In sum, the method for extracting aglycon from the root of Chinese clematis that the present invention is provided is conducive to total saposins to hydrolyze, and discharges glycosides
Unit and side-chain radical, gained aglycon purity is high, and process is simple, low cost, can large-scale application in industrialized production.
Claims (10)
1. it is a kind of from the root of Chinese clematis extract aglycon method, it is characterised in that comprise the following steps：
(1) root of Chinese clematis is crushed, crosses 60~80 mesh sieves, to 70%~95% ethanol is added in powder, carried in 30~50 DEG C of backflows
1~2h is taken, cold filtration obtains total saponin extracts；Wherein, root of Chinese clematis powder quality and ethanol volume ratio are 1~3:40~50；
(2) to the hydrochloric acid solution that concentration is 1~5mol/L is added in step (1) gained total saponin extracts, in 60~100 DEG C of water
0.5~2.5h of solution, obtains hydrolyzate；Wherein, acid solution and total saponin extracts volume ratio are 1~5:1~3；
(3) it is by volume 1:1 ratio is extracted 2~3 times to petroleum ether is added in step (2) gained hydrolyzate, separates oil
Ether layer and water layer, then be by volume 1~1.5:1~2 ratio is extracted 2~3 times, in 60 to ethyl acetate is added in water layer
Concentrated below DEG C, enriched product is obtained；
(4) dissolved to addition methyl alcohol in enriched product, then separated with preparation liquid phase, Fractional Collections efflux obtains aglycon.
2. it is according to claim 1 from the root of Chinese clematis extract aglycon method, it is characterised in that：Second described in step (1)
Alcohol mass concentration is 70% ethanol.
3. it is according to claim 1 from the root of Chinese clematis extract aglycon method, it is characterised in that：Prestige described in step (1)
Medicine xiaolingxian powder quality is 1 with ethanol volume ratio:50.
4. it is according to claim 1 from the root of Chinese clematis extract aglycon method, it is characterised in that：Acid described in step (2)
Liquid is hydrochloric acid, sulfuric acid, oxalic acid or boric acid.
5. it is according to claim 1 from the root of Chinese clematis extract aglycon method, it is characterised in that：Water described in step (2)
Solution condition is：In 100 DEG C, concentration are for the acid solution of 2mol/L, 1h is hydrolyzed.
6. it is according to claim 1 from the root of Chinese clematis extract aglycon method, it is characterised in that：Acid described in step (2)
Liquid is 1.2 with total saposins volume ratio:1.
7. it is according to claim 1 from the root of Chinese clematis extract aglycon method, it is characterised in that：Second described in step (3)
Acetoacetic ester is 1 with water layer volume ratio:1.
8. it is according to claim 1 from the root of Chinese clematis extract aglycon method, it is characterised in that：Made described in step (4)
It is for liquid phase separation gradient：
Mobile phase is water and methyl alcohol, and column temperature is room temperature, 0~30min, 60%~90% methyl alcohol, 40%~10% water；Flow velocity 5mL/
min。
9. the aglycon that the method that aglycon is extracted from the root of Chinese clematis described in any one of claim 1~8 is prepared.
10. application of the aglycon described in claim 9 in medicine for treating rheumatoid arthritis preparation.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115671123A (en) * | 2021-07-21 | 2023-02-03 | 苏州凯祥生物科技有限公司 | Application of clematis root saponin in preparation of purine-lowering medicine |
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| CN101216462A (en) * | 2007-12-29 | 2008-07-09 | 广州中医药大学科技产业园有限公司 | Clematis chinensis medicinal materials effective ingredient content determination method |
| CN105954383A (en) * | 2016-04-22 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Determination method for oleanolic acid and hederagenin in clematis root |
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2017
- 2017-03-10 CN CN201710139465.9A patent/CN106905405A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1900106A (en) * | 2005-07-20 | 2007-01-24 | 北京凯瑞创新医药科技有限公司 | Method for preparing Chinese medicine extract and quality control method |
| CN101216462A (en) * | 2007-12-29 | 2008-07-09 | 广州中医药大学科技产业园有限公司 | Clematis chinensis medicinal materials effective ingredient content determination method |
| CN105954383A (en) * | 2016-04-22 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Determination method for oleanolic acid and hederagenin in clematis root |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115671123A (en) * | 2021-07-21 | 2023-02-03 | 苏州凯祥生物科技有限公司 | Application of clematis root saponin in preparation of purine-lowering medicine |
| CN115671123B (en) * | 2021-07-21 | 2024-03-22 | 苏州凯祥生物科技有限公司 | Application of clematis root saponin in preparation of purine-reducing medicament |
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