CN108484711B - A method of preparing gypenoside LI - Google Patents
A method of preparing gypenoside LI Download PDFInfo
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- CN108484711B CN108484711B CN201810243192.7A CN201810243192A CN108484711B CN 108484711 B CN108484711 B CN 108484711B CN 201810243192 A CN201810243192 A CN 201810243192A CN 108484711 B CN108484711 B CN 108484711B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
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- C07J17/00—Normal steroids containing carbon, hydrogen, halogen or oxygen, having an oxygen-containing hetero ring not condensed with the cyclopenta(a)hydrophenanthrene skeleton
- C07J17/005—Glycosides
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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Abstract
The invention discloses a kind of methods for preparing gypenoside LI, this method is to belong to but the heart seed gynostemma pentaphylla Gynostemma cardiospermum Cogn.ex Oliv of different subgenus substitutes gynostemma pentaphylla Gynostemma pentaphyllum (Thunb.) Makino as raw material, a large amount of gypenoside LVI can be prepared with extraction separation and purification, XLVI, L, LI, damulin A and damulin B, gypenoside LVI, XLVI, L, LI, the content of damulin A and damulin B in heart seed gynostemma pentaphylla Gynostemma cardiospermum Cogn.ex Oliv leaf is in gynostemma pentaphylla Gynostem respectively 10-50 times of content in mapentaphyllum (Thunb.) Makino leaf；And heart seed gynostemma pentaphylla Gynostemma cardiospermum Cogn.ex Oliv is not commercialized, unrestrained field be nobody shows any interest in all over the fields, and cost can be ignored.
Description
Technical field
The invention belongs to biomedicine fields, and in particular to a method of prepare gypenoside LI.
Background technique
Gynostemma pentaphylla Gynostemmapentaphyllum (Thunb.) Makino also known as Herb Gynostemmae Pentaphylli, Radix Rhodiolae, Herba Gynostemmatis
Deng being the herbaceous perennial vine plant of Curcurbitaceae gynostemma pentaphyllum genus, be mainly grown in the area on the south the Qinling Mountains and the Changjiang river in China.
It makees edible wild herbs use first recorded in the herbal for Relief of Famines of the Ming Dynasty, starts for it to be used as medicine with the name of " Japanese Cayratia Herb " in Compendium of Material Medica.
" the strong pharmacy of China ": " tri- two-way of Tong Tiao, clearing heat and detoxicating, cough-relieving apophlegmatic.For chronic bronchitis, virus hepatitis, renal plevis kidney
Inflammation, gastroenteritis, diarrhea, hypertension, arteriosclerosis, hyperlipidemia, ulcerative carbuncle pyogenic infections, snake bite ".Main chemical compositions in gynostemma pentaphylla
For saponin(e and polysaccharide, in addition also contain a small amount of flavone compound, terpene, organic acid, protein, vitamin, fat, fiber
Equal ingredients and zinc, copper, magnesium, iron, manganese, selenium and other trace elements.Gynostemma pentaphylla has antitumor, hypoglycemic, anti-aging, anti-liver fiber
The pharmacological actions such as change, principle active component gypenoside excessive use is also without side-effects, thus in health food and novel
There is huge application prospect on drug research and development, is a kind of new medical and edible dual purpose plant resource.
The saponin constituent contained in gynostemma pentaphylla is numerous, study it is more, active preferably have gypenoside LVI, XLVI, L,
LI, damulin A (DamulinA) and damulin B (Damulin B).Wherein, gypenoside LVI, XLVI content is higher, other
Four kinds are the extremely low rare saponin(e of content (for the converted product of gypenoside LVI, XLVI).
Currently, gypenoside LVI, XLVI are obtained by raw material extraction separation and purification of gynostemma pentaphylla, gypenoside L, LI,
Damulin A and damulin B obtained using the gynostemma pentaphylla that is processed by heating as raw material extraction separation and purification (document:
Determination by UPLC-MS of four dammaranetype saponins from heat-processed
Gynostemma pentaphyllum；Bioscience,Biotechnology,andBiochemistry,2014；Vol.78,
No.2,311-316).Gypenoside LVI, XLVI, L, LI, damulin A and damulin B is prepared as raw material using gynostemma pentaphylla to exist
Two o'clock is insufficient:
First, gynostemma pentaphylla price is relatively high, at high cost.Since State Scientific and Technological Commission in 1986 in Spark Program strand
Indigo plant is classified as the first place of " rare traditional Chinese medicine " leaved for development, and the market price of gynostemma pentaphylla is just obvious to go up.
Second, it is very low not heat gypenoside L, LI, damulin A and damulin B in the gynostemma pentaphylla of processing, separates pure
It is big to change difficulty；Heating processing is bothersome, and gypenoside L, LI, the content of damulin A and damulin B and asynchronous increasing after heating
Add, acid extraction is difficult to control (above-mentioned citation can also embody this phenomenon).
Gynostemma pentaphyllum genus shares 2 subgenus, 13 kind of 2 mutation, and 2 subgenus are gynostemma pentaphylla subgenus, beak fruit rattan subgenus, above-mentioned gynostemma pentaphylla
Gynostemmapentaphyllum (Thunb.) Makino is one of gynostemma pentaphylla subgenus (document: gynostemma plant
Categorizing system and distribution, Acta Phytotaxonomica Sinica, 1995).Research invention, gynostemma plant all contain gynostemma pentaphylla soap substantially
Glycosides, and type is essentially identical, but the content difference of specific gypenoside is larger in the different plants of the category.Originate from Hu Beixi
The heart seed gynostemma pentaphylla Gynostemma cardiospermum Cogn.ex Oliv in portion, Southern Shaanxi and Sichuan belongs to beak fruit rattan
Subgenus, being mainly characterized by fruit is capsule, and top is cracked along ventral suture when mature, has the 3 pieces of beak styles harbored, other features
It is then almost the same with gynostemma pentaphylla Gynostemmapentaphyllum (Thunb.) Makino.Open strand is not yet had been reported that at present
Blue saponin(e LVI, XLVI, L, LI, damulin A, B are in heart seed gynostemma pentaphylla Gynostemma cardiospermum Cogn.ex
Content in Oliv is significantly higher than gynostemma pentaphylla Gynostemmapentaphyllum (Thunb.) Makino.
Summary of the invention
It is an object of that present invention to provide a kind of methods for preparing gypenoside LI.
Above-mentioned purpose is achieved through the following technical solutions:
Gypenoside LVI, XLVI, L, LI, damulin A and damulin B preparation method include the following steps:
Step S1 collects the leaf of heart seed gynostemma pentaphylla Gynostemma cardiospermum Cogn.ex Oliv, dries in the shade,
With ethanol water heating and refluxing extraction, filtered through gauze, merging filtrate is concentrated into no alcohol taste；
The extracting solution for being concentrated into no alcohol taste is splined on D101 large pore resin absorption column by step S2, and it is 1 that resin path height, which compares:
10, sample resin accounts for resin total amount 1/10 is mixed, wet method dress post mixes resin loading；First with 30% ethyl alcohol of 10BV with 10BV/h's
Flow velocity elution removal of impurities, then eluted with 85% ethyl alcohol of 10BV with the flow velocity of 10BV/h, 3-10BV eluent is collected, no alcohol is concentrated into
Taste obtains total saposins aqueous solution；
Total saposins aqueous solution is adjusted pH value to 6.0, chitosan/attapulgite clay compound, room temperature is added by step S3
Stirring is stood, filtering, collects filtrate, adjusts pH value to neutrality, freeze-drying obtains purification total saposins powder；
Purification total saposins powder is splined on normal phase silicagel column by step S4, and silica gel diameter height compares for 1:10, is mixed sample silica gel and is accounted for silicon
The 1/10 of glue total amount, dry column-packing mix silica gel loading；Successively with two that volume ratio is 20:1:2,10:1:2,5:1:2,2:1:2
Chloromethanes/methanol/acetone mixed solvent elutes 10BV, 6BV, 5BV, 3BV with the flow-rate gradient elution of 12BV/h respectively；
It is dry to collect 20:1:2 methylene chloride/methanol/acetone elution 7-8BV, 9-10BV eluent concentration respectively by step S5
It is dry to obtain damulin B, damulin A；10:1:2 methylene chloride/methanol/acetone elution 3-4BV, 5-6BV eluent is collected respectively
Concentrate drying obtains gypenoside L, gypenoside LI；5:1:2 methylene chloride/methanol/acetone elution 4-5BV is collected to wash
De- liquid is concentrated and dried to obtain gypenoside XLVI；It is dense to collect 2:1:2 methylene chloride/methanol/acetone elution 2-3BV eluent
Contracting is dried to obtain gypenoside LVI.
Preferably, chitosan/attapulgite clay compound is the preparation method comprises the following steps: 1g chitosan is dissolved in 100mL mass fraction
To obtain chitosan sol in 1% aqueous acetic acid, 8g attapulgite clay is added into the colloidal sol, stirring at normal temperature 48h is quiet
Upper solution is poured out after setting 2h, 50 DEG C of residue drying, grinding, drying.
Preferably, step S1 ethanol water concentration expressed in percentage by volume is 75%.
Preferably, the solid-to-liquid ratio that step S1 is extracted is 1:20.
Preferably, 50g chitosan/attapulgite clay compound is added in 1L total saposins aqueous solution in step S3.
Preferably, step S3 is stirred for 24 hours after chitosan/attapulgite clay compound is added, and is filtered after standing 2h.
Preferably, step S3 hydrochloric acid and ammonium hydroxide adjust pH.
The technology of the present invention advantage:
1, the present invention is to belong to but the heart seed gynostemma pentaphylla Gynostemma cardiospermum Cogn.ex of different subgenus
Gynostemma pentaphylla Gynostemmapentaphyllum (Thunb.) Makino is as raw material for Oliv substitution, can be with extraction separation and purification system
It is standby to obtain a large amount of gypenoside LVI, XLVI, L, LI, damulin A and damulin B, gypenoside LVI, XLVI, L, LI, reach
The content difference of the wooden woods A and damulin B in heart seed gynostemma pentaphylla Gynostemma cardiospermum Cogn.ex Oliv leaf
It is 10-50 times of the content in gynostemma pentaphylla Gynostemmapentaphyllum (Thunb.) Makino leaf；And heart seed strand
Blue Gynostemma cardiospermum Cogn.ex Oliv is not commercialized, and unrestrained field be nobody shows any interest in all over the fields, and cost can neglect
Slightly.
2, step S3 of the present invention refines total saposins aqueous solution with chitosan/attapulgite clay compound, effectively
The impurity in total saposins is reduced, subsequent normal phase silica gel column chromatography technique is greatlied simplify, product purity is high.
Detailed description of the invention
Fig. 1 is the efficient liquid phase chromatographic analysis spectrogram of step S2 total saposins aqueous solution；
Fig. 2 is the efficient liquid phase chromatographic analysis spectrogram that step S3 refines total saposins powder；
Fig. 3 is the efficient liquid phase chromatographic analysis spectrogram for the damulin B that silica gel chromatography obtains；
Fig. 4 is the efficient liquid phase chromatographic analysis spectrogram for the damulin A that silica gel chromatography obtains；
Fig. 5 is the efficient liquid phase chromatographic analysis spectrogram for the gypenoside L that silica gel chromatography obtains；
Fig. 6 is the efficient liquid phase chromatographic analysis spectrogram for the gypenoside LI that silica gel chromatography obtains；
Fig. 7 is the efficient liquid phase chromatographic analysis spectrogram for the gypenoside XLVI that silica gel chromatography obtains；
Fig. 8 is the efficient liquid phase chromatographic analysis spectrogram for the gypenoside LVI that silica gel chromatography obtains.
Specific embodiment
Essentiality content of the invention is specifically introduced below with reference to embodiment, but it will be appreciated by those skilled in the art that not
Protection scope of the present invention should be confined to these specific embodiments.
One, experimental material
The leaf of heart seed gynostemma pentaphylla Gynostemma cardiospermum Cogn.ex Oliv is collected from Hubei Shiyan City room
County, the leaf of gynostemma pentaphylla Gynostemmapentaphyllum (Thunb.) Makino make after drying in the shade collected from Hunan Shaoyang Suining
With.
Chitosan/attapulgite clay compound is the preparation method comprises the following steps: it is 1% that 1g chitosan, which is dissolved in 100mL mass fraction,
Chitosan sol is obtained in aqueous acetic acid, and 8g attapulgite clay, stirring at normal temperature 48h, after standing 2h are added into the colloidal sol
Upper solution is poured out, 50 DEG C of residue drying, grinding, drying.
Different concentration ethanol refers both to the ethanol water of different volumes percentage concentration.
Two, experimental method
1, the preparation of gypenoside LVI, XLVI, L, LI, damulin A and damulin B
Include the following steps:
Step S1 collects the leaf of heart seed gynostemma pentaphylla Gynostemma cardiospermum Cogn.ex Oliv, dries in the shade,
The ethanol water heating and refluxing extraction for being 75% with concentration expressed in percentage by volume, solid-to-liquid ratio 1:20 are extracted 3 times, each 2h, gauze
Filtering, merging filtrate are concentrated into no alcohol taste；
The extracting solution for being concentrated into no alcohol taste is splined on D101 large pore resin absorption column by step S2, and it is 1 that resin path height, which compares:
10, sample resin accounts for resin total amount 1/10 is mixed, wet method dress post mixes resin loading；First with 30% ethyl alcohol of 10BV with 10BV/h's
Flow velocity elution removal of impurities, then eluted with 85% ethyl alcohol of 10BV with the flow velocity of 10BV/h, 3-10BV eluent is collected, no alcohol is concentrated into
Taste obtains total saposins aqueous solution；
It is compound that chitosan/attapulgite clay is added in total saposins aqueous solution salt acid for adjusting pH value to 6.0 by step S3
50g chitosan/attapulgite clay compound is added in object, 1L total saposins aqueous solution, and stirring for 24 hours, is filtered after standing 2h, collects filter
Liquid, ammonium hydroxide adjust pH value to neutrality, and freeze-drying obtains purification total saposins powder；
Purification total saposins powder is splined on normal phase silicagel column by step S4, and silica gel diameter height compares for 1:10, is mixed sample silica gel and is accounted for silicon
The 1/10 of glue total amount, dry column-packing, mix silica gel loading (purification total saposins powder dissolved with methanol after with mix sample silica gel and mix
It is even, dry, purification total saposins powder and the mass ratio 1:1 for mixing sample silica gel)；It is successively 20:1:2,10:1:2,5:1 with volume ratio:
2, methylene chloride/methanol/acetone mixed solvent of 2:1:2 is with the flow-rate gradient elution of 12BV/h, elute respectively 10BV, 6BV,
5BV,3BV；
It is dry to collect 20:1:2 methylene chloride/methanol/acetone elution 7-8BV, 9-10BV eluent concentration respectively by step S5
It is dry to obtain damulin B, damulin A；10:1:2 methylene chloride/methanol/acetone elution 3-4BV, 5-6BV eluent is collected respectively
Concentrate drying obtains gypenoside L, gypenoside LI；5:1:2 methylene chloride/methanol/acetone elution 4-5BV is collected to wash
De- liquid is concentrated and dried to obtain gypenoside XLVI；It is dense to collect 2:1:2 methylene chloride/methanol/acetone elution 2-3BV eluent
Contracting is dried to obtain gypenoside LVI.
2, efficient liquid phase chromatographic analysis condition
Chromatograph: LC-20ADXR high-pressure pump；SPD-M20A diode array ultraviolet-visible detector；CTO-20AC column
Incubator；CBM-20A system controller；SIL-20ACXR autosampler；
Chromatographic column: Agilent ZORBAX Extend-C18 (250mm × 4.6mm, 5 μm)；
Mobile phase A phase: water (contains 5/10000ths tetrahydrofurans)；
Mobile phase B phase: acetonitrile (contains 5/10000ths tetrahydrofurans)；
Elution program: 0-3min, 20%B phase；3-15min, 20% → 40%B phase；15-30min, 40% → 80%B phase；
Flow velocity: 1.0mL/min；
Column temperature: 30 DEG C；
Detection wavelength: 203nm；
Sample volume: 10 μ L.
Three, experimental result
It takes step S2 total saposins aqueous solution to dilute 5 times and is used as high performance liquid chromatography sample introduction solution, step S3 is taken to refine total soap
Glycosides powder uses the mobile phase of initial proportion to be dissolved into the solution of 0.5mg/mL as high performance liquid chromatography sample introduction solution.Fig. 1 is step
The efficient liquid phase chromatographic analysis spectrogram of rapid S2 total saposins aqueous solution, Fig. 2 are the high-efficient liquid phase color that step S3 refines total saposins powder
Spectrum analysis spectrogram.From Fig. 1,2 as it can be seen that total saposins aqueous solution complicated component obtained by step S2, step S3 refine impurity in total saposins
Ingredient greatly reduces, and illustrates that chitosan/attapulgite clay compound can the total soap of effective Adsorption under the conditions of 6.0 pH
Impurity component in glycosides aqueous solution.By removal of impurities, facilitate the technology difficulty for reducing subsequent silica gel column chromatography.
Purification total saposins obtained after step S4, S5 silica gel column chromatography separating purification gypenoside LVI, XLVI, L,
LI, damulin A and damulin B monomer.Fig. 3 is the efficient liquid phase chromatographic analysis spectrum for the damulin B that silica gel chromatography obtains
Figure, Fig. 4 are the efficient liquid phase chromatographic analysis spectrogram for the damulin A that silica gel chromatography obtains, and Fig. 5 is silica gel chromatography
The efficient liquid phase chromatographic analysis spectrogram of obtained gypenoside L, Fig. 6 are the gypenoside LI that silica gel chromatography obtains
Efficient liquid phase chromatographic analysis spectrogram, Fig. 7 is the high performance liquid chromatography of gypenoside XLVI that silica gel chromatography obtains
Analysis of spectra, Fig. 8 are the efficient liquid phase chromatographic analysis spectrogram for the gypenoside LVI that silica gel chromatography obtains.From Fig. 3-8
As it can be seen that gypenoside LVI, XLVI, L, LI, damulin A and damulin B purity are very high, 95% or more.By a silicon
Gypenoside LVI, XLVI, L, LI, damulin A and the damulin B of such high-purity can be prepared in plastic column chromatography, mainly
Have benefited from step S3 chitosan/attapulgite clay compound refining and edulcoration.
The present invention has the advantage that
The present invention is to belong to but the heart seed gynostemma pentaphylla Gynostemma cardiospermum Cogn.ex of different subgenus
Gynostemma pentaphylla Gynostemmapentaphyllum (Thunb.) Makino is as raw material for Oliv substitution, can be with extraction separation and purification system
It is standby to obtain a large amount of gypenoside LVI, XLVI, L, LI, damulin A and damulin B, gypenoside LVI, XLVI, L, LI, reach
The content difference of the wooden woods A and damulin B in heart seed gynostemma pentaphylla Gynostemma cardiospermum Cogn.ex Oliv leaf
It is 12,11,45,37,42,55 times of the content in gynostemma pentaphylla Gynostemmapentaphyllum (Thunb.) Makino leaf
(dried leaf of two kinds of gynostemma pentaphylla, solid ratio 1:40, ultrasonic 40min, filtering, then with height directly operating method: are extracted with methanol
Effect liquid phase chromatogram method analyzes filtrate, according to the peak face of gypenoside LVI, XLVI, L, LI, damulin A and damulin B
Its content ratio in two kinds of filtrates is roughly calculated in product ratio)；And heart seed gynostemma pentaphylla Gynostemma cardiospermum
Cogn.ex Oliv is not commercialized, and unrestrained field be nobody shows any interest in all over the fields, and cost of material can be ignored.
Step S3 of the present invention refines total saposins aqueous solution with chitosan/attapulgite clay compound, effectively drops
Impurity in low total saposins, greatlies simplify subsequent normal phase silica gel column chromatography technique, and product purity is high.
Claims (6)
1. a kind of method for preparing gypenoside LI, which comprises the steps of:
Step S1 collects heart seed gynostemma pentaphyllaGynostemma cardiospermumCogn. the leaf of ex Oliv, dries in the shade, and uses second
Alcohol solution heating and refluxing extraction, filtered through gauze, merging filtrate are concentrated into no alcohol taste；
The extracting solution for being concentrated into no alcohol taste is splined on D101 large pore resin absorption column by step S2, and resin path height compares for 1:10, is mixed
Sample resin accounts for the 1/10 of resin total amount, and wet method dress post mixes resin loading；First washed with 30% ethyl alcohol of 10BV with the flow velocity of 10BV/h
It removes miscellaneous, then is eluted with 85% ethyl alcohol of 10BV with the flow velocity of 10BV/h, collect 3-10BV eluent, be concentrated into no alcohol taste and obtain
Total saposins aqueous solution；
Total saposins aqueous solution is adjusted pH value to 6.0, chitosan/attapulgite clay compound is added, room temperature stirs by step S3
It mixes, stand, filter, collect filtrate, adjust pH value to neutrality, freeze-drying obtains purification total saposins powder；
Purification total saposins powder is splined on normal phase silicagel column by step S4, and silica gel diameter height compares for 1:10, and mixing sample silica gel, to account for silica gel total
The 1/10 of amount, dry column-packing mixes silica gel loading；It is successively methylene chloride/methanol/acetone of 20:1:2,10:1:2 with volume ratio
Mixed solvent elutes 10BV, 6BV with the flow-rate gradient elution of 12BV/h respectively；
Step S5 collects 10:1:2 methylene chloride/methanol/acetone elution 5-6BV eluent and is concentrated and dried to obtain gynostemma pentaphylla soap
Glycosides LI；
Wherein, chitosan/attapulgite clay compound is the preparation method comprises the following steps: it is 1% that 1g chitosan, which is dissolved in 100 mL mass fractions,
Chitosan sol is obtained in aqueous acetic acid, and 8g attapulgite clay, stirring at normal temperature 48h, after standing 2h are added into the colloidal sol
Upper solution is poured out, 50 DEG C of residue drying, grinding, drying.
2. according to the method described in claim 1, it is characterized by: step S1 ethanol water concentration expressed in percentage by volume is 75%.
3. according to the method described in claim 2, it is characterized by: the solid-to-liquid ratio that step S1 is extracted is 1:20.
4. according to the method described in claim 1, it is characterized by: in step S3 1L total saposins aqueous solution be added 50g chitosan/
Attapulgite clay compound.
5. according to the method described in claim 4, it is characterized by: chitosan/attapulgite clay compound is added in step S3
After stir for 24 hours, stand 2h after filter.
6. according to the method described in claim 1, it is characterized by: step S3 hydrochloric acid and ammonium hydroxide adjust pH.
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| PCT/CN2018/093947 WO2019178980A1 (en) | 2018-03-23 | 2018-07-01 | Method for preparing gynostemma pentaphylla makino saponin lvi, xlvi, l, li, damulin a or damulin b |
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| CN1008821B (en) * | 1986-06-25 | 1990-07-18 | 安康地区科学技术委员会 | Making method of natural blue total saponin |
| CN1068575A (en) * | 1992-03-11 | 1993-02-03 | 孙文基 | The production technique of long stalk gynostemma laxum |
| KR20030023232A (en) * | 2001-09-12 | 2003-03-19 | 주식회사 뉴젠팜 | Method of extracting saponin from Panax ginseng or Gynostemma pentaphyllum and foods containing the extracted saponin therefrom |
| CN102552371B (en) * | 2012-01-16 | 2013-11-13 | 中央民族大学 | Gynostemma pentaphylla extractive and application thereof to preparing medicine for treating tumor |
| CN102579471B (en) * | 2012-01-16 | 2013-12-11 | 中央民族大学 | Applications of four gypenoside compounds in preparation of medicament for treating tumors |
| CN102603849A (en) * | 2012-02-10 | 2012-07-25 | 厦门华侨亚热带植物引种园 | Gynostemma pentaphylla secondary saponin, preparation method and applications thereof |
| CN103169725A (en) * | 2013-01-29 | 2013-06-26 | 中央民族大学 | Gynostemma pentaphyllum extract and application thereof in preparation of medicament for treating tumor |
| CN103908486A (en) * | 2014-03-17 | 2014-07-09 | 中国农业大学 | Preparing method of gynostemma pentaphyllum extraction product rich in gypenosides |
| CN103923149B (en) * | 2014-04-15 | 2017-02-15 | 厦门华侨亚热带植物引种园 | Gynostemma pentaphylla saponin XLV Ed and preparation method thereof |
| CN104327148A (en) * | 2014-10-24 | 2015-02-04 | 中央民族大学 | Compounds with antitumor activity, and preparation method and application thereof |
| KR101773081B1 (en) * | 2015-12-31 | 2017-08-30 | 국가식품클러스터지원센터 | Dolwoe fermented extracts comprising saponins as an active functional food ingredient and preparation method thereof |
| CN107126452A (en) * | 2016-02-26 | 2017-09-05 | 上海中医药大学附属曙光医院 | Gypenosides and preparation method thereof |
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