CN100446781C - Method for preparing general saponin of golden Chinese gentian and application - Google Patents
Method for preparing general saponin of golden Chinese gentian and application Download PDFInfo
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- CN100446781C CN100446781C CNB2006101294239A CN200610129423A CN100446781C CN 100446781 C CN100446781 C CN 100446781C CN B2006101294239 A CNB2006101294239 A CN B2006101294239A CN 200610129423 A CN200610129423 A CN 200610129423A CN 100446781 C CN100446781 C CN 100446781C
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Abstract
A process for preparing the general saponin of golden gentian used for treating the ulcer in digestive tract includes such steps as extracting in alcohol and then in ethylacetate and n-butanol, vacuum concentrating chromatography by macroreticular resin, gradient eluting, and vacuum concentrating.
Description
Technical field
The present invention relates to a kind of preparation method and application thereof of general saponin of golden Chinese gentian, relate to particularly that a kind of cost is lower, environmental pollution is little and be suitable for the preparation method of general saponin of golden Chinese gentian of suitability for industrialized production and the application in anti-peptic ulcer drug.
Background technology
Conyza is a Compositae Radix Asteris family plant, and the whole world has 80-100 kind, mainly is distributed in the torrid zone and the subtropical zone in east, the Western Hemisphere.China has 10 kinds approximately at present, and such as conyza blinii, Radix Conyzae sumatrensis, Herba Erigerontis aceris, Conyza bonariensis (L.) Crong. and Herba Erigerontis Canadensis etc., major part originates in south and area, the west and south.Wherein conyza blinii is the dry herb of Herba Acroptili repentis in the Conyza plant (Conyza blinii L é vl.), experiment showed, chemical compounds such as containing Diterpenes, flavonoid, sesquiterpenoids, triterpenes and saponins in the conyza blinii.The inventor is engaged in the research of conyza blinii effective ingredient for a long time, and finds first that by experiment conyza blinii can obtain general saponin of golden Chinese gentian through the processing of the following step.Described treatment step comprises: (1) uses 60% alcohol reflux 1 time then with 95% alcohol reflux 2 times; (2) with silicagel column 95% ethanol extraction is carried out chromatographic isolation, and use petroleum ether, chloroform, ethyl acetate and methanol-eluted fractions successively; (3) utilize ultrasound wave that methanol-eluted fractions thing and 60% alcohol extractive are handled with acetone, merge insoluble matter then and through D101 resin column chromatography, water, 30%, 70% and 95% ethanol elution obtain general saponin of golden Chinese gentian with 70% ethanol elution thing concentrating under reduced pressure.But, as mentioned above, need to use silica gel that the ethanol extraction of conyza blinii is handled in the step 2 of this preparation method, because silica gel can't reclaim after using, so it can cause serious pollution to environment, and the organic solvent kind of using in this step is more, thereby handle long and complicated operating process of required time, so not only can increase production cost, and be unsuitable for suitability for industrialized production.Particularly carry out can causing dead absorption in the processing procedure at the ethanol extraction that utilizes silica gel to conyza blinii, the result causes reaching the low yield below 1.2%.
Summary of the invention
In order to address the above problem, to the object of the present invention is to provide that a kind of cost is lower, environmental pollution is little and be suitable for the preparation method of the general saponin of golden Chinese gentian of suitability for industrialized production.
Another object of the present invention is to provide the application of a kind of general saponin of golden Chinese gentian in treatment digestive tract ulcer disease medicament.
In order to achieve the above object, the preparation method of general saponin of golden Chinese gentian provided by the invention comprises the following step that carries out in order:
(1) will be through the conyza blinii of powder essence heating and refluxing extraction 2 times in 90%～dehydrated alcohol, each 2 hours, after the filtration filtering residue was also filtered with 55%～65% alcohol heating reflux extraction in 2 hours, twice filtrate is merged, be evaporated to ethanol then and volatilize fully;
(2) be 10～20g/100ml with above-mentioned concentrated solution with distilled water diluting to concentration, then in separatory funnel with equivalent ethyl acetate extraction 4 times to remove impurity, and water layer decompression steamed to ethyl acetate volatilize fully, in separatory funnel, use the equivalent n-butanol extraction repeatedly more afterwards, until extraction fully, the butanol extraction liquid concentrating under reduced pressure after will merging at last and obtain thick saponin;
(3) above-mentioned thick saponin is water-soluble and through macroporous resin D101 column chromatography, water, 30% ethanol, 70% ethanol and 95% ethanol carry out gradient elution successively then, at last 70% ethanol elution thing concentrating under reduced pressure can be obtained general saponin of golden Chinese gentian.
The yield of described general saponin of golden Chinese gentian is 1.6～3.0%.
The preparation method of general saponin of golden Chinese gentian provided by the invention need not to use silicagel column that the ethanol extraction of conyza blinii is handled, thereby can not produce environmental pollution, and the interest rate height.In addition, it is less to handle the organic solvent kind that ethanol extraction adopted, thereby the processing time is short and operating process is simple, not only can reduce production costs like this, and is suitable for suitability for industrialized production.In addition, the anti-alimentary tract ulcer of general saponin of golden Chinese gentian is active clear and definite, thereby can be applicable to treat in the medicine of digestive tract ulcer disease.
The specific embodiment
Contain 16 kinds of triterpene saponin componds in the general saponin of golden Chinese gentian, the title and the molecular formula of these chemical compounds are respectively: Chinese liquor grass saponin A, C
62H
100O
30Chinese liquor grass saponin B, C
67H
108O
34Chinese liquor grass saponin C, C
68H
110O
34Chinese liquor grass saponin D, C
73H
118O
40Chinese liquor grass saponin E, C
73H
118O
40Chinese liquor grass saponin F, C
68H
109O
36Chinese liquor grass saponin H, C
68H
109O
36Chinese liquor grass saponin I, C
63H
102O
30Chinese liquor grass saponin J, C
63H
102O
31Chinese liquor grass saponin K, C
68H
110O
35Chinese liquor grass saponin L, C
69H
112O
36Chinese liquor grass saponin M, C
67H
108O
34Chinese liquor grass saponin N, C
62H
100O
30Chinese liquor grass saponin O, C
68H
110O
35Chinese liquor grass saponin P, C
62H
100O
30Chinese liquor grass saponin Q, C
67H
108O
34General saponin of golden Chinese gentian is a kind of sundown powder, has stronger hygroscopicity, is soluble in ethanol, methanol, water, is insoluble to acetone, chloroform, ethyl acetate; Can form abundant foam after its aqueous solution jolting, and yield is 1.6～3.0%.
Embodiment 1:
To extract 2 times with 95% alcohol heating reflux through the conyza blinii herb 17kg that pulverizes, each 2 hours, after the filtration filtering residue was extracted 2 hours and filtered with 60% alcohol heating reflux, twice filtrate is merged, be evaporated to ethanol then and volatilize fully.With above-mentioned concentrated solution with distilled water diluting to 11 liter, this moment, concentration was 17g/100ml, then in separatory funnel with equivalent ethyl acetate extraction 4 times to remove impurity, and water layer decompression steamed to ethyl acetate volatilize fully, afterwards again in separatory funnel with equivalent n-butanol extraction 7 times, the butanol extraction liquid concentrating under reduced pressure after will merging at last and obtain thick saponin 602g.Above-mentioned thick saponin is water-soluble and at twice through macroporous resin D101 column chromatography (1610g, chromatographic column: 10 * 88cm), water, 30% ethanol, 70% ethanol, 95% ethanol carry out gradient elution successively then, at last 70% ethanol elution thing is concentrated and obtain general saponin of golden Chinese gentian 283g, yield is 1.7%.
With general saponin of golden Chinese gentian 150g through silica gel column chromatography (2500g, chromatographic column: 10 * 110cm), carry out gradient elution with chloroform-methanol-water then and obtain three component LGT, QGT, the BGT of general saponin of golden Chinese gentian, mainly comprise Chinese liquor grass saponin I, Chinese liquor grass saponin B, Chinese liquor grass saponin D respectively.
The general saponin of golden Chinese gentian pharmacodynamic study:
Experimental gastric ulcer model due to the employing ligation rat pylorus is studied the effect of general saponin of golden Chinese gentian anti-alimentary tract ulcer.
1. to the influence of rat model gastric mucosa ulcer:
The general saponin of golden Chinese gentian of the present invention's preparation can obviously reduce the area of gastric ulcer under the dosage of 50mg/kg/d, obviously reduce the gastric ulcer index, shows that general saponin of golden Chinese gentian has good protective effect to the rat gastric ulcer due to the ligation pylorus; Its three component LGT, QGT, BGT also can obviously reduce the area of gastric ulcer, but effect weakens.
2. to the influence of rat model gastric juice amount and gastric acidity:
The general saponin of golden Chinese gentian of the present invention's preparation can obviously suppress the secretion of gastric juice under the dosage of 50mg/kg/d, obviously reduce the total gastric acid in the gastric juice, obviously suppresses the output of total acid; Its three component LGT, QGT, BGT also can obviously suppress the secretion of gastric juice and gastric acid, but effect weakens.
3. to the influence of malonaldehyde, hydroxy radical in the rat model gastric mucosa:
The general saponin of golden Chinese gentian of the present invention preparation can obviously reduce the content of malonaldehyde and hydroxy radical in the gastric mucosa under the dosage of 50mg/kg/d; Its three component LGT, QGT, BGT also can obviously reduce the content of malonaldehyde and hydroxy radical in the gastric mucosa, but effect weakens.
Sum up above pharmacodynamic study result, general saponin of golden Chinese gentian has good anti-alimentary tract ulcer activity, the antiulcer activity of its three component LGT, QGT, BGT weakens than general saponin of golden Chinese gentian, but the different effect of performance in the anti-alimentary tract ulcer, wherein the effect that MDA and OH generate in the QGT inhibition gastric mucosa is strong, BGT inhibition gastric juice and the excretory effect of gastric acid are strong, and the effect of LGT is placed in the middle.Therefore general saponin of golden Chinese gentian can be used as the active component of treatment digestive tract ulcer medicine.
Embodiment 2:
With dry and through the conyza blinii 62g that pulverizes with 94% alcohol heating reflux extraction 2 times, each 2 hours; After the filtration filtering residue was extracted 2 hours and filtered with 61% alcohol heating reflux, twice filtrate is merged, be evaporated to ethanol then and volatilize fully.With above-mentioned concentrated solution with distilled water diluting to 100ml, this moment, concentration was 11g/100ml, then in separatory funnel with equivalent ethyl acetate extraction 4 times to remove impurity, and water layer is evaporated to ethyl acetate volatilizees fully, afterwards again in separatory funnel with equivalent n-butanol extraction 7 times, the butanol extraction liquid concentrating under reduced pressure after will merging at last and obtain thick saponin 3.5g.Above-mentioned thick saponin is water-soluble and through macroporous resin D101 column chromatography, water, 30% ethanol, 70% ethanol, 95% ethanol carry out gradient elution successively then, at last 70% ethanol elution thing concentrating under reduced pressure can be obtained general saponin of golden Chinese gentian 1.8g, yield is 2.9%.
Embodiment 3:
With dry and extract 2 times with 98% alcohol heating reflux through the conyza blinii 1kg that pulverizes, each 2 hours, after the filtration filtering residue was extracted 2 hours and filtration with 63% alcohol heating reflux, with twice filtrate merging, be evaporated to ethanol then and volatilize fully.With above-mentioned concentrated solution with distilled water diluting to 1000ml, this moment, concentration was 14g/100ml, then in separatory funnel with equivalent ethyl acetate extraction 4 times to remove impurity, and water layer is evaporated to ethyl acetate volatilizees fully, afterwards again in separatory funnel with equivalent n-butanol extraction 7 times, the butanol extraction liquid concentrating under reduced pressure after will merging at last and obtain thick saponin 45.9g.Above-mentioned thick saponin is water-soluble and through macroporous resin D101 column chromatography, water, 30% ethanol, 70% ethanol, 95% ethanol carry out gradient elution successively then, at last 70% ethanol elution thing concentrating under reduced pressure can be obtained general saponin of golden Chinese gentian 19.3g, yield is 1.9%.
Claims (2)
1, a kind of preparation method of general saponin of golden Chinese gentian is characterized in that: the preparation method of described general saponin of golden Chinese gentian comprises the following step that carries out in order:
(1) will be through the conyza blinii of powder essence heating and refluxing extraction 2 times in 90%～dehydrated alcohol, each 2 hours, after the filtration filtering residue was also filtered with 55%～65% alcohol heating reflux extraction in 2 hours, twice filtrate is merged, be evaporated to ethanol then and volatilize fully;
(2) be 10～20g/100ml with above-mentioned concentrated solution with distilled water diluting to concentration, then in separatory funnel with equivalent ethyl acetate extraction 4 times to remove impurity, and water layer decompression steamed to ethyl acetate volatilize fully, in separatory funnel, use the equivalent n-butanol extraction repeatedly more afterwards, until extraction fully, the butanol extraction liquid concentrating under reduced pressure after will merging at last and obtain thick saponin;
(3) above-mentioned thick saponin is water-soluble and through macroporous resin D101 column chromatography, water, 30% ethanol, 70% ethanol and 95% ethanol carry out gradient elution successively then, at last 70% ethanol elution thing concentrating under reduced pressure can be obtained general saponin of golden Chinese gentian.
2, the preparation method of general saponin of golden Chinese gentian according to claim 1 is characterized in that: the yield of described general saponin of golden Chinese gentian is 1.6～3.0%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101933964A (en) * | 2010-09-03 | 2011-01-05 | 天津大学 | Application of conyza blinii total saponins for preparing anti-neoplastic drug |
Families Citing this family (6)
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| CN101284861B (en) * | 2008-05-04 | 2010-08-18 | 天津大学 | Triterpenoid saponin compounds, preparation method and use |
| CN104606273A (en) * | 2014-10-27 | 2015-05-13 | 天津科技大学 | Gastric mucosal protective agent containing Conyza blinii total saponin and application thereof in preparation of preparations preventing and treating ethanol induced gastrorrhagia |
| CN105287782A (en) * | 2015-10-19 | 2016-02-03 | 李敬 | Cherry leaf extract for treating gastric ulcer and preparation method of cherry leaf extract |
| CN106237065A (en) * | 2016-08-25 | 2016-12-21 | 神威药业集团有限公司 | A kind of pharmaceutical composition and preparation method thereof |
| CN112274571A (en) * | 2020-12-02 | 2021-01-29 | 西安医学院 | Antibacterial hydrogel suitable for diabetic foot ulcer and preparation method thereof |
| CN113679748A (en) * | 2021-06-07 | 2021-11-23 | 重庆威迪特药业有限责任公司 | Preparation and detection method and application of saponin in conyza blinii |
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2006
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Non-Patent Citations (6)
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| Four new triterpenoid saponins from Conyza blinii.. Su Y, Guo D, Guo H, Liu J, Zheng J, Koike K, Nikaido T.J Nat Prod.,Vol.64 No.1. 2001 |
| Four new triterpenoid saponins from Conyza blinii.. Su Y, Guo D, Guo H, Liu J, Zheng J, Koike K, Nikaido T.J Nat Prod.,Vol.64 No.1. 2001 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101933964A (en) * | 2010-09-03 | 2011-01-05 | 天津大学 | Application of conyza blinii total saponins for preparing anti-neoplastic drug |
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