CN1068575A - The production technique of long stalk gynostemma laxum - Google Patents
The production technique of long stalk gynostemma laxum Download PDFInfo
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- CN1068575A CN1068575A CN 92101498 CN92101498A CN1068575A CN 1068575 A CN1068575 A CN 1068575A CN 92101498 CN92101498 CN 92101498 CN 92101498 A CN92101498 A CN 92101498A CN 1068575 A CN1068575 A CN 1068575A
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Abstract
The present invention is a production technique of extracting total saponin from longstipe gynostemma herb.Adopt resin adsorption method, the raw material decocting is extracted, decocting liquid is removed non-saponin class impurity by polyamide column, then by macroporous resin column absorption, ethanol elution, the elutriant drying handle finished product: perhaps in decocting liquid, add flocculation agent, make non-saponin class impurity generate precipitation, filtrate is carried out resin absorption and ethanol elution again, and elutriant is again by anion-exchange column, the effluent liquid drying handle finished product.The removal of impurity of the present invention is effective, and is simple for process, quality of finished product good, and the extraction yield height is suitable for suitability for industrialized production.
Description
The present invention is a production technique of extracting total saponin from longstipe gynostemma herb.
Cucurbitaceae genus gynostemma, the whole world have 13 kinds, and China has 11 kinds, and longstipe gynostemma herb (Gynostemma Longips G.Y.Wu.) is different from other gynostemma plant, and flavor is extremely bitter, has another name called " Rhizome or herb of Fiveleaf Gynostemma ", and it is one of exclusive gynostemma pentaphylla kind of China.Longstipe gynostemma herb mainly is distributed in Qin crust mountain area and Hubei one band, and is bigger in the standing stock in each county, south, Shaanxi.At present, also there is not the people that the chemical ingredients and the pharmacological action of longstipe gynostemma herb are studied both at home and abroad.The present inventor studies longstipe gynostemma herb, extracts to obtain long stalk gynostemma laxum, and it has been carried out system's separation, also wherein two compounds has been carried out the structure evaluation.The structure of these two compounds is referring to Fig. 1,2,3, when the R among Fig. 1 is structure among Fig. 2, called after longstipe gynostemma herb saponin A, when the R among Fig. 1 is structure among Fig. 3, called after longstipe gynostemma herb saponin B, this part content was published on 221～222 pages of " Chinese chemical journal " (Chinese Chemical letters) 1991 23 phases of volume.By among the figure as can be seen longstipe gynostemma herb be different from other gynostemma pentaphylla kind, its contained saponin component is mainly pentacyclic triterpene.More to the research report of gynostemma pentaphylla (Gynostemma Pentaphtnum Mark.) at present, this gynostemma pentaphylla kind flavor is sweet, have another name called " Pentapanax leschenaultii ", Japanese bamboo Ben Changsong furthers investigate its chemical ingredients, therefrom isolate more than 50 saponin and other constituents, wherein four kinds identical with ginsenoside, main component is a tetracyclic triterpenes.Show that according to experiment the reducing blood lipid of longstipe gynostemma herb saponin is better than gypenoside, so its extraction is of great value.The extraction process of long stalk gynostemma laxum can be used for reference the extraction process of total gypenosides.In prior art, the clear 57-58699 of Japanese Patent adopts resin adsorption method to extract total gypenosides, technical process is: gynostemma pentaphylla raw material water decocts, decocting liquid adsorbs by macroporous resin column then, use the methanol-eluted fractions macroporous resin column again, elutriant is removed non-saponin class impurity by alumina column, obtains finished product after last meoh eluate drying is handled.The operation that Japanese Patent is removed non-saponin class impurity mainly is that elutriant passes through alumina column, alumina column and non-saponin class impurity have good avidity, make the impurity elimination effect comparatively desirable, finished product color and luster good (contain total saponin and be about 70%) with panoxadiol calculating, but the alumina column irreversible adsorption is serious, the saponin rate of loss accounts for 30%, has reduced extraction yield.In addition, alumina column is difficult to reuse because activation is complicated, is not suitable for suitability for industrialized production.Another critical defect of this technology has been to use the methyl alcohol of toxic effect, has proposed " preparation method of total gypenosides " in order to improve this shortcoming Chinese patent CN86104409, has replaced methanol-eluted fractions with ethanol in this patent, has eliminated the public hazards pollution.But this patent is avoided the problem of removing non-saponin class impurity in the above-mentioned Japanese Patent, it omitted by this step of alumina column, the new technological process of removing non-saponin class impurity is not proposed again, therefore, the finished product that extracts with this method is actually Herb Gynostemmae Pentaphylli total glycosides, rather than total saponin, owing in general glycoside, contain non-saponin class impurity, make that the purity of finished product and color and luster are all very bad.
The objective of the invention is to propose a kind of production technique that is suitable for the long stalk gynostemma laxum extraction, and in this technology, overcome the shortcoming in the existing gynostemma pentaphylla extraction process, not only make impurity elimination effective, make technological process simple simultaneously.
Solution of the present invention is as follows: adopt the resin adsorption method production technique, this technology comprises following process, the raw material decocting is extracted, extracting solution adsorbs by macroporous resin column, wash macroporous resin column with Diluted Alcohol and remove polysaccharide and partial pigment impurity in the adsorptive, with medical ethanol wash-out macroporous resin column, the elutriant drying is handled, and gets finished product.Use for reference aforesaid method and extract long stalk gynostemma laxum, wherein raw material adopts the longstipe gynostemma herb over-ground part, draw according to research the longstipe gynostemma herb over-ground part, the total saponin of longstipe gynostemma herb over-ground part accounts for 7%, major part is various impurity, these impurity mainly are: polysaccharide, chlorophyll, flavones and phenolic acid compound, and wherein flavones and phenolic acid compound belong to non-saponin class impurity, and its content is more.Therefore, impurities removal is a major issue in the extraction process of long stalk gynostemma laxum.Adopt above-mentioned technology can remove polysaccharide and partial pigment impurity in the raw material, but can't remove non-saponin class impurity.Owing to contain a large amount of non-saponin class impurity in the raw material, the existence of arborescens thing in the raw material in addition, make the decocting liquid of this raw material so limpid unlike the decocting liquid of gynostemma pentaphylla, but it is thick to be black, if this decocting liquid directly carries out resin absorption, then the black dope in the liquid will the wrapped resin periphery, weakens or lose the absorption property of resin, the finished product extraction yield is reduced, and finished product purity and color and luster are also extremely bad; Simultaneously, this decocting liquid also is not easy by resin column very much, if pass through by force, must use recoil method, destroys the post bed, and decompression is passed through; In addition, resin also poisons easily, has reduced its repeat performance.According to this situation, the decocting liquid of raw material must be removed the processing of non-saponin class impurity earlier.The method that the present invention proposes has two kinds: the one, and decocting liquid by polyamide column, makes non-saponin class impurity be removed by the polymeric amide adsorption by hydrogen bond earlier, and then carries out following operation such as resin absorption, obtains finished product; The 2nd, in decocting liquid, add flocculation agent, make non-saponin class impurity generate precipitation, filtrate is carried out resin absorption and ethanol elution technology again, exist inorganic anion in the resulting ethanol eluate, for removing mineral ion, ethanol eluate is by anion-exchange column, and effluent liquid carries out drying treatment more then, gets finished product.
Good impurity removing effect of the present invention, final product quality is more satisfactory, and impurity removal process is simple, does not lose saponin.The polyamide column activation is simple, can use repeatedly, is suitable for suitability for industrialized production.
Describe in detail according to embodiment below.
The structure iron of Fig. 1, longstipe gynostemma herb saponin.
The structure iron of Fig. 2, longstipe gynostemma herb saponin A.
The structure iron of Fig. 3, longstipe gynostemma herb saponin B.
Embodiment 1,100 kilograms in longstipe gynostemma herb over-ground part hay, and about 250 kilograms of water decocts three times, each 1 hour, decocting liquid merged, filtered while hot, and filtrate is passed through polyamide column, column chromatography polymeric amide (60～40 order) 40 kilograms, 20 kilograms of glass wools, layering dress post.The polymeric amide flow velocity is slower, adds glass wool and can improve flow velocity.Make effluent liquid pass through macroporous resin column then, i.e. macroporous resin D
10140 kilograms on type, or macroporous resin D
101: D
201=1: 3, extract is attracted in the macroporous resin column, elder generation is cleaned with 20% ethanol, removes polysaccharide and partial pigment impurity, washes the effluent liquid color always and shoals, using the medical ethanol wash-out, after being washed till the effluent liquid evaporate to dryness, till the water-soluble no obvious foam, elutant decompression recycling ethanol then, take out pine at last, obtain buff powder.
Embodiment 2, and 100 kilograms in longstipe gynostemma herb over-ground part hay is handled through decocting similarly to Example 1, add flocculation agent 200～500 grams then in the decocting liquid, add to no obvious sediment regeneration, and selected flocculation agent can be aluminum chloride (AlCl
3), calcium oxide (CaO), ferrous sulfate (FeSO
4), this example adopts aluminum chloride, aluminum ion can generate precipitation with non-saponin class impurity combination well, solution filtered while hot then, filtrate is carried out resin absorption and the ethanol elution technology identical with embodiment 1, ethanol eluate is removed the negatively charged ion (as: Cl in the elutriant by anion-exchange column (being strong basicity negative resin or AB-8 type resin) then
-), effluent liquid carries out drying treatment again and obtains the finished product identical in quality with embodiment 1 then.
More than the yield of two embodiment be 1～2%.Calculate with longstipe gynostemma herb saponin A, total saponin content is 60～90%.
Can find out further that by above-mentioned two embodiment product yield height of the present invention, purity are good, technological process is simple.
Claims (3)
1, the production technique of long stalk gynostemma laxum, adopt the resin adsorption method production technique, this technology has following technological process, the raw material decocting is extracted, decocting liquid adsorbs by macroporous resin column, washes macroporous resin column with Diluted Alcohol and removes polysaccharide and partial pigment impurity in the adsorptive, with medical ethanol wash-out macroporous resin column, the elutriant drying handle finished product, it is characterized in that:
A, raw material are the over-ground parts of longstipe gynostemma herb (Gynostemma Longips G.Y.Wu.),
B, decocting liquid pass through polyamide column earlier, and then carry out following operations such as resin absorption, obtain finished product, perhaps add flocculation agent in the decocting liquid, filter, filtrate is carried out operations such as resin absorption and ethanol elution again, and resulting ethanol eluate passes through anion-exchange column, effluent liquid carries out drying treatment more then, gets finished product.
2, production technique as claimed in claim 1 is characterized in that: described polyamide column is 60～40 orders, and adorns posts with 40 kilograms of polymeric amide, 20 kilograms of glass wool layerings.
3, as claim 1,2 described production technique, it is characterized in that: described flocculation agent is aluminum chloride (AlCl
3), calcium oxide (CaO), ferrous sulfate (FeSO
4).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92101498 CN1068575A (en) | 1992-03-11 | 1992-03-11 | The production technique of long stalk gynostemma laxum |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92101498 CN1068575A (en) | 1992-03-11 | 1992-03-11 | The production technique of long stalk gynostemma laxum |
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| CN1068575A true CN1068575A (en) | 1993-02-03 |
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| CN 92101498 Pending CN1068575A (en) | 1992-03-11 | 1992-03-11 | The production technique of long stalk gynostemma laxum |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1317295C (en) * | 2003-01-16 | 2007-05-23 | 北京大学安康药物研究院 | Preparation method of gynostemma pentaphylia total saponin |
| CN1317294C (en) * | 2003-01-16 | 2007-05-23 | 北京大学安康药物研究院 | Preparation method of gynostemma pentaphylia total saponin |
| CN108484711A (en) * | 2018-03-23 | 2018-09-04 | 娄志春 | A method of preparing gypenoside LI |
| CN108484713A (en) * | 2018-03-23 | 2018-09-04 | 娄志春 | A method of preparing gypenoside L |
| CN116098929A (en) * | 2023-03-07 | 2023-05-12 | 陕西嘉禾生物科技股份有限公司 | Method for extracting gynostemma pentaphylla total saponin from gynostemma pentaphylla |
-
1992
- 1992-03-11 CN CN 92101498 patent/CN1068575A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1317295C (en) * | 2003-01-16 | 2007-05-23 | 北京大学安康药物研究院 | Preparation method of gynostemma pentaphylia total saponin |
| CN1317294C (en) * | 2003-01-16 | 2007-05-23 | 北京大学安康药物研究院 | Preparation method of gynostemma pentaphylia total saponin |
| CN108484711A (en) * | 2018-03-23 | 2018-09-04 | 娄志春 | A method of preparing gypenoside LI |
| CN108484713A (en) * | 2018-03-23 | 2018-09-04 | 娄志春 | A method of preparing gypenoside L |
| CN116098929A (en) * | 2023-03-07 | 2023-05-12 | 陕西嘉禾生物科技股份有限公司 | Method for extracting gynostemma pentaphylla total saponin from gynostemma pentaphylla |
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