CN1869056A - Method of extracting and separating ginseng saponine mixture from ginseng leaf - Google Patents
Method of extracting and separating ginseng saponine mixture from ginseng leaf Download PDFInfo
- Publication number
- CN1869056A CN1869056A CN 200610093612 CN200610093612A CN1869056A CN 1869056 A CN1869056 A CN 1869056A CN 200610093612 CN200610093612 CN 200610093612 CN 200610093612 A CN200610093612 A CN 200610093612A CN 1869056 A CN1869056 A CN 1869056A
- Authority
- CN
- China
- Prior art keywords
- ginsenoside
- aqueous solution
- ginseng
- wash
- mixture
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Steroid Compounds (AREA)
Abstract
A process for extracting and separating ginsenoside mixture from ginseng leaf includes such steps as preparing extract from ginseng leaf, adsorbing with macroreticular resin, eluting with low-concentration and high-concentration organic solvents to obtain two mixtures of ginsenosides, and recrystallizing or chromatography with alumina column to obtain more mixtures of ginsenosides.
Description
Technical field
The present invention relates to the mixture that the various ginsenoside of extraction separation is formed from the Ginseng Leaf is panaxsaponin mixture's method, belongs to the Natural Medicine Chemistry research field.
Background technology
The Ginseng Leaf is the dry leave of genseng (Panax ginseng C.A.Mey.), and gather autumn, dries or dries; Gas delicate fragrance, mildly bitter flavor and sweet; Have tonifying Qi, beneficial lung drives away summer heat, the function of promoting the production of body fluid; Be used for the qi-asthenia cough, hot summer weather is fidgety, and Tianjin wound is thirsty, and the head is unclear, and four limbs are tired.
Up to the present people get multiple ginsenoside from the Ginseng Leaf, and that wherein often mentions has a ginsenoside Rg
1, ginsenoside Re, ginsenoside Rb
1, ginsenoside Rb
2, ginsenoside Rb
3, Ginsenoside Rc, Ginsenoside Rd etc.
Summary of the invention
The mixing saponin(e of being made up of different ginsenosides is that usually said group saponine has different biological activitys.Such as by ginsenoside Rb
1, ginsenoside Rb
2, ginsenoside Rb
3, composition such as Ginsenoside Rc, Ginsenoside Rd glycol group ginsenoside have central inhibitory action, antih(a)emolysin; And mainly by ginsenoside Re, ginsenoside Rg
1Then have central excitation effect and hemolytic action Deng the triol group ginsenoside of forming.
The present invention to provide a kind of from the Ginseng Leaf the various panaxsaponin mixture's of extraction separation novel method, especially contain ginseng saponin F
1, ginseng saponin F
2And the panaxsaponin mixture's of N-Fe novel method, be to provide from the Ginseng Leaf extraction separation more specifically mainly by ginsenoside Re and ginsenoside Rg
1Composition and ginsenoside Re's content is greater than the ginsenoside Rg
1The panaxsaponin mixture; Mainly by ginsenoside Re and ginsenoside Rg
1Form and the ginsenoside Rg
1Content greater than ginsenoside Re's panaxsaponin mixture; Mainly by ginseng saponin F
1, the ginsenoside Rg
2, ginseng saponin F
2, N-Fe, Ginsenoside Rd, ginsenoside Rb
2, Ginsenoside Rc, ginsenoside Rb
1With ginsenoside Rb
3The panaxsaponin mixture who forms; Mainly by ginseng saponin F
1And ginsenoside Rg
2The panaxsaponin mixture who forms; Mainly by ginseng saponin F
2, the panaxsaponin mixture that forms of N-Fe, Ginsenoside Rd; Mainly by ginseng saponin F
1, the ginsenoside Rg
2, ginseng saponin F
2, the panaxsaponin mixture that forms of N-Fe, Ginsenoside Rd; Mainly by Ginsenoside Rd, ginsenoside Rb
2, Ginsenoside Rc, ginsenoside Rb
1With ginsenoside Rb
3The panaxsaponin mixture's who forms method.The panaxsaponin mixture who obtains can be used for pharmaceutical compositions, protective foods and ginsenoside monomer.Concrete technical scheme is as follows.
Extraction separation Ginseng Leaf total saponins from the Ginseng Leaf at present, the most frequently used method is the macroporous adsorbent resin method.Be that Ginseng Leaf's boiling is extracted, extracting solution is crossed absorption with macroporous adsorbent resin, wash, and the ethanolic soln wash-out, elutriant reclaims solvent, obtains Ginseng Leaf's total saponins.
Normally used in above-mentioned elution process is the alcoholic acid aqueous solution of higher concentration, so all saponin(e is eluted, what obtain is Ginseng Leaf's total saponins.We are by discovering, if transfer concentration of ethanol lower, promptly use the alcoholic acid aqueous solution (such as the 18%) wash-out of low concentration, with silica gel thin-layer chromatography (developping agent: propyl carbinol: ethyl acetate: water=4: 1: 5, the upper strata) checks the composition that is eluted, find only be equivalent to the ginsenoside Rg
1Locate to occur two spots with the ginsenoside Re, also do not occur simultaneously the peak of other ginsenoside in its high-efficient liquid phase chromatogram, that illustrate that the aqueous ethanolic solution of lower concentration elutes is the ginsenoside Rg
1And ginsenoside Re.Aqueous ethanolic solution wash-out with a large amount of lower concentrations detects less than the ginsenoside Rg to elutriant
1Spot with the ginsenoside Re that is to say the ginsenoside Rg
1Carry out wash-out with the aqueous ethanolic solution of higher concentration with ginsenoside Re's wash-out again after fully, at this moment other ginsenosides are eluted.Check the composition that is eluted by the high concentration ethanol aqueous solution with silica gel thin-layer chromatography (developping agent: propyl carbinol: ethyl acetate: water=4: 1: 5, upper strata), find except Ginsenoside Rd, ginsenoside Rb
2, ginsenoside Rb
1, Ginsenoside Rc and ginsenoside Rb
3Outside spot, be equivalent to the ginsenoside Rg
1Still occur and the ginsenoside Rg with ginsenoside Re's position
1Spot with ginsenoside Re's same color.In order to understand fully that these two spots are the ginsenoside Rg
1And the ginsenoside Re, we utilize high performance liquid chromatography to verify, found that they are not the ginsenoside Rgs
1And ginsenoside Re.Illustrate that these two spots are and the ginsenoside Rg
1With identical other compositions of ginsenoside Re's Rf value (with propyl carbinol: ethyl acetate: water=4: 1: 5, upper strata are under the condition of developping agent).In order to understand fully that what composition these two spots are, we utilize the method for silica gel column chromatography and ODS column chromatography, separate, purifying above-mentioned two compositions, and pass through
13C-NMR has identified its chemical structure.Found that the ginsenoside Rg
1The spot that the place occurs is a ginseng saponin F
2, the spot of locating to occur the ginsenoside Re is a N-Fe.From above-mentioned result of study, we have obtained as drawing a conclusion.Be except there being the ginsenoside Rg who often mentions among the Ginseng Leaf
1, ginsenoside Re, Ginsenoside Rd, ginsenoside Rb
2, Ginsenoside Rc, ginsenoside Rb
1With ginsenoside Rb
3Also there is ginseng saponin F outward
2And N-Fe; Ginsenoside Rg when developping agent is (propyl carbinol: ethyl acetate: water=4: 1: 5, upper strata)
1And ginseng saponin F
2, ginsenoside Re and N-Fe the Rf value in full accord.The more important thing is that above-mentioned result of study tells us, utilize the aqueous ethanolic solution of macroporous adsorbent resin and lower concentration, can be the ginsenoside Rg
1And ginseng saponin F
2, ginsenoside Re and N-Fe separately, that is to say with extract of Radix Ginseng leaf or Ginseng Leaf's total saponins with absorption with macroporous adsorbent resin after with the aqueous ethanolic solution wash-out of lower concentration, ginsenoside Rg
1Eluted with the ginsenoside Re, and the ginseng saponin F approaching with their polarity
2Still be attracted on the resin with N-Fe.We also find the ginsenoside Rg in addition
1(ginseng saponin F
2) also there is a comparatively significantly spot in the top of spot, through silica gel column chromatography and ODS column chromatography for separation, purifying and pass through
13The C-NMR Spectrum Analysis finds that it is a ginseng saponin F
1Then we are to the ginseng saponin F in Ginseng Leaf and the Ginseng Leaf's total saponins
1, ginseng saponin F
2, N-Fe content measure.Found that ginseng saponin F in Ginseng Leaf and the Ginseng Leaf's total saponins
1, ginseng saponin F
2, N-Fe content is higher, ginseng saponin F especially
1, ginseng saponin F
2The concrete outcome of measuring is to contain ginseng saponin F among the Ginseng Leaf
1About 0.5%, ginseng saponin F
2About 0.4%, N-Fe about 0.1%; And contain ginseng saponin F in Ginseng Leaf's total saponins
1About 7%, the ginsenoside Rg
1About 10%, ginseng saponin F
2About 6%, ginsenoside Re about 20%, N-Fe about 1%, Ginsenoside Rd about 10%, ginsenoside Rb
2About 4%, Ginsenoside Rc about 4%, ginsenoside Rb
1About 1% and ginsenoside Rb
3About 0.8%, also contain a small amount of ginsenoside Rg simultaneously
2And other people join saponin(e.
There is bibliographical information from the Ginseng Leaf, to separate in the past and identified ginseng saponin F
1, ginseng saponin F
2And N-Fe.But up to now, it is believed that in Ginseng Leaf or the Ginseng Leaf's total saponins and mainly contain the ginsenoside Rg
1, ginsenoside Re, Ginsenoside Rd, ginsenoside Rb
2, Ginsenoside Rc, ginsenoside Rb
1With ginsenoside Rb
3, about ginseng saponin F
1, ginseng saponin F
2, N-Fe research report seldom.That is to say, it is believed that up to now Ginseng Leaf's total saponins is the ginsenoside Rg
1, ginsenoside Re, Ginsenoside Rd, ginsenoside Rb
2, Ginsenoside Rc, ginsenoside Rb
1With ginsenoside Rb
3Mixture.But we are by discovering that Ginseng Leaf's total saponins is a ginseng saponin F
1, the ginsenoside Rg
1, the ginsenoside Rg
2, ginseng saponin F
2, ginsenoside Re, N-Fe, Ginsenoside Rd, ginsenoside Rb
2, Ginsenoside Rc, ginsenoside Rb
1With ginsenoside Rb
3Mixture.
So far we have found among the Ginseng Leaf except containing the ginsenoside Rg
1, ginsenoside Re, Ginsenoside Rd, ginsenoside Rb
2, Ginsenoside Rc, ginsenoside Rb
1With ginsenoside Rb
3Also contain relatively large ginseng saponin F outward
1, ginseng saponin F
2, N-Fe; Ginseng Leaf's total saponins should be a ginseng saponin F
1, the ginsenoside Rg
1, the ginsenoside Rg
2, ginseng saponin F
2, ginsenoside Re, N-Fe, Ginsenoside Rd, ginsenoside Rb
2, Ginsenoside Rc, ginsenoside Rb
1With ginsenoside Rb
3Mixture; These are found to be the mixture of the various different ginsenosides of forming of extraction separation from the Ginseng Leaf, and promptly the panaxsaponin mixture lays a good foundation.We have invented following panaxsaponin mixture and have especially contained ginseng saponin F on this basis
1, ginseng saponin F
2, N-Fe panaxsaponin mixture's preparation method.Concrete technical scheme is as follows.
With extract of Radix Ginseng leaf (Ginseng Leaf's total saponins) with behind the absorption with macroporous adsorbent resin earlier with low-concentration ethanol aqueous solution wash-out, at this moment ginsenoside Rg
1Eluted with the ginsenoside Re, and the ginsenoside Rg approaching with their polarity
2, ginseng saponin F
2With N-Fe and polarity than they little ginseng saponin Fs
1, polarity is than their big Ginsenoside Rds, ginsenoside Rb
2, ginsenoside Rb
1, Ginsenoside Rc, ginsenoside Rb
3Deng still being attracted on the resin.Therefore use the alcoholic acid aqueous solution of low concentration with the ginsenoside Rg
1With ginsenoside Re's wash-out fully after, use the aqueous ethanolic solution wash-out of higher concentration again, just can be ginsenoside Re, ginsenoside Rg
1With other ginsenosides separately.
Studies show that further except ethanol, the aqueous solution of organic solvents such as methyl alcohol, acetone, n-propyl alcohol, Virahol or the aqueous solution of their mixture also have identical effect.That is to say Ginseng Leaf's boiling is extracted that extracting solution is crossed absorption with macroporous adsorbent resin, use the aqueous solution wash-out of the above-mentioned organic solvent of low concentration earlier, just ginsenoside Re and the ginsenoside Rg that elute this moment
1, other ginsenosides still are attracted on the resin.With ginsenoside Re and ginsenoside Rg
1Use the aqueous solution wash-out of the above-mentioned organic solvent of higher concentration after wash-out is complete again, what at this moment elute is to comprise ginseng saponin F
1, N-Fe and ginseng saponin F
2At other interior ginsenosides, thus can be with the ginsenoside separated into two parts among the Ginseng Leaf, i.e. ginsenoside Re and ginsenoside Rg
1Mixture (panaxsaponin mixture A) and ginseng saponin F
1, the ginsenoside Rg
2, ginseng saponin F
2, N-Fe, Ginsenoside Rd, ginsenoside Rb
2, Ginsenoside Rc, ginsenoside Rb
1With ginsenoside Rb
3Mixture (panaxsaponin mixture B).
Only contain ginsenoside Re and ginsenoside Rg among the panaxsaponin mixture A
1, wherein ginsenoside Re's content is greater than the ginsenoside Rg
1Content, approximately be the ginsenoside Rg
12-3 doubly.
Contain ginseng saponin F among the panaxsaponin mixture B
1, the ginsenoside Rg
2, ginseng saponin F
2, ginsenoside Rb
1, ginsenoside Rb
2, ginsenoside Rb
3, Ginsenoside Rc, Ginsenoside Rd and N-Fe, do not contain or contain the ginsenoside Re and the ginsenoside Rg of small amount of residual
1Whether residual ginsenoside Re and ginsenoside Rg
1, relevant with the aqueous solution wash-out degree of the organic solvent of using low concentration, if wash-out is thorough, do not contain ginsenoside Re and ginsenoside Rg among the panaxsaponin mixture B
1
For ginsenoside Re and ginsenoside Rg under the wash-out
1, the concentration of the aqueous solution of used ethanol, methyl alcohol, acetone, n-propyl alcohol, Virahol or their mixture can not be too high.If the excessive concentration of the aqueous solution of the ethanol that uses, methyl alcohol, acetone, n-propyl alcohol, Virahol then glycol group ginsenosides such as Ginsenoside Rd, Ginsenoside Rc under can wash-out; But can not be low excessively, if crossing low meeting wash-out, the concentration of the aqueous solution of used ethanol, methyl alcohol, acetone, n-propyl alcohol, Virahol or their mixture do not descend ginsenoside Re and ginsenoside Rg
1The concentration that we find them generally between 15%-40% for well, 15%-20% preferably.Because the optimum concn of ethanol or methyl alcohol or acetone or n-propyl alcohol or Virahol is relevant with the polarity of the macroporous adsorbent resin of use, therefore finally should select suitable concentration according to the polarity height of macroporous adsorbent resin.
Ginsenoside Re and ginsenoside Rg
1Be dissolved in after eluting in the aqueous solution of organic solvent of lower concentration.This solution is difficult to concentrate, and has adopted following method in order to address this problem the present invention.Be about to contain ginsenoside Re and ginsenoside Rg
1The direct or water of the aqueous solution cross macroporous adsorbent resin again after adding dilution less, at this moment be dissolved in ginsenoside Re and ginsenoside Rg in the solution
1Will be attracted on the macroporous adsorbent resin again, and then get final product with reclaiming solvent behind the high concentration ethanol wash-out.
Macroporous adsorbent resin described in the present invention can or have the polymeric adsorbent of other trades mark of same or similar performance with macroporous adsorbent resins commonly used such as AB-8, D4020,860021, D101, D102, D103, HP-20.
The present invention further utilizes the method for recrystallization to obtain the ginsenoside Rg from panaxsaponin mixture A
1Content mainly contain ginsenoside Re and ginsenoside Rg greater than ginsenoside Re's content
1The panaxsaponin mixture; Utilize the method for alumina column chromatography from panaxsaponin mixture B, to obtain the simple more panaxsaponin mixture of several compositions.Specific as follows.
With the aqueous solution recrystallization of panaxsaponin mixture A water or alcohol, this moment, ginsenoside Re's crystallization was separated out, and can obtain ginsenoside Re and mother liquor respectively after the filtration.Mother liquor is crossed absorption with macroporous adsorbent resin again after gac or decolorizing resin decolouring, ethanol elution reclaims ethanol, and obtaining new panaxsaponin mixture is panaxsaponin mixture C.These characteristics of mixing saponin(e are ginsenoside Rgs wherein
1Content greater than the ginsenoside Re, approximately be the ginsenoside Re 2-3 doubly, just in time opposite with panaxsaponin mixture A.
With alumina column on the panaxsaponin mixture B, the aqueous solution wash-out of the organic solvent of first water or lower concentration, what at this moment elute is ginseng saponin F
1And ginsenoside Rg
2(may comprise a small amount of remaining ginsenoside Rg
1And ginsenoside Re), thus obtain mainly to contain ginseng saponin F
1And ginsenoside Rg
2The mixing saponin(e be panaxsaponin mixture D; With ginseng saponin F
1Use the aqueous solution wash-out of the organic solvent of high density after wash-out is complete again, what at this moment elute is ginseng saponin F
2, N-Fe and Ginsenoside Rd, thereby obtain mainly to contain ginseng saponin F
2, N-Fe and Ginsenoside Rd the panaxsaponin mixture be panaxsaponin mixture E, use the aqueous solution wash-out of tetrahydrofuran (THF) at last, be Ginsenoside Rd, ginsenoside Rb under the wash-out at this moment
2, Ginsenoside Rc, ginsenoside Rb
1With ginsenoside Rb
3Thereby, obtain mainly to contain Ginsenoside Rd, ginsenoside Rb
2, Ginsenoside Rc, ginsenoside Rb
1With ginsenoside Rb
3The mixing saponin(e be panaxsaponin mixture F; Perhaps with alumina column on the panaxsaponin mixture B, directly using the aqueous solution wash-out of the organic solvent of high density, under the wash-out is ginseng saponin F at this moment
1, the ginsenoside Rg
2, ginseng saponin F
2, N-Fe and Ginsenoside Rd (may comprise a small amount of remaining ginsenoside Rg
1And ginsenoside Re), thus obtain mainly to contain ginseng saponin F
1, the ginsenoside Rg
2, ginseng saponin F
2, N-Fe and Ginsenoside Rd the mixing saponin(e be panaxsaponin mixture G, use the aqueous solution wash-out of tetrahydrofuran (THF) at last, be Ginsenoside Rd, ginsenoside Rb under the wash-out at this moment
2, Ginsenoside Rc, ginsenoside Rb
1With ginsenoside Rb
3, clump and obtain mainly to contain Ginsenoside Rd, ginsenoside Rb
2, Ginsenoside Rc, ginsenoside Rb
1With ginsenoside Rb
3The mixing saponin(e be panaxsaponin mixture F.Said organic solvent is meant ethanol or methyl alcohol or acetone or n-propyl alcohol or Virahol or their mixture in the above-mentioned alumina column chromatography.
Wash-out ginseng saponin F in the above-mentioned alumina column chromatography process
1, the ginsenoside Rg
2Preferably making water, is the aqueous solution wash-out words of ethanol or methyl alcohol or acetone or n-propyl alcohol or Virahol or their mixture if use the aqueous solution of the organic solvent of lower concentration, and its concentration should be controlled at and be unlikely to ginseng saponin F
2, N-Fe and Ginsenoside Rd elute and be advisable, and generally should be lower than 40%; The wash-out ginseng saponin F
2, N-Fe should use the ethanol of higher concentration or the aqueous solution of methyl alcohol or acetone or n-propyl alcohol or Virahol or their mixture, its concentration generally between 40%-95%, is preferably in about 60%; The concentration of the aqueous solution of tetrahydrofuran (THF) is preferably in about 50% between 35%-85%; The aluminum oxide that uses is neutral alumina preferably.
Embodiment
Embodiment 1
7 kilograms of Ginseng Leafs, boiling is extracted three times, each amount of water is respectively 18,12,10 times of Ginseng Leaf's weight, decocting time is respectively 2,1.5,1 hours, merge decoction liquor, cross the D4020 absorption with macroporous adsorbent resin, water washes down, and 18% ethanol elution detects less than ginsenoside Re and ginsenoside Rg to elutriant
1After use 85% ethanol elution instead and detect less than Ginsenoside Rd and ginsenoside Rb to the elutriant
1Till (silica gel thin-layer chromatography, propyl carbinol: ethyl acetate: water=4: 1: 5, the upper strata, 10% sulfuric acid spraying, 105 ℃ of heating colour developings, below identical).18% ethanol eluate is crossed the AB-8 absorption with macroporous adsorbent resin again, detects less than ginsenoside Re and ginsenoside Rg to elutriant with 85% ethanol elution then
1, elutriant reclaims ethanol, gets panaxsaponin mixture A 308 grams.Detect through HPLC, contain the ginsenoside Rg
19.68%, the ginsenoside Re 22.61%.85% ethanol eluate directly reclaims ethanol, obtains panaxsaponin mixture B 326 grams.Detect through HPLC, contain ginsenoside Rb
11.92%, ginsenoside Rb
23.98%, ginsenoside Rb
30.48%, Ginsenoside Rc 4.41%, Ginsenoside Rd 8.63%, ginseng saponin F
15.97%, ginseng saponin F
26.19%, N-Fe 1.78%.
Panaxsaponin mixture A 300 grams add 600 ml water heating for dissolving, place, and precipitation is filtered, water washing and precipitating, and drying gets ginsenoside Re's 102.2 grams.Detect through HPLC, contain the ginsenoside Rg
11.21%, the ginsenoside Re 96.54%, do not contain other ginsenoside.Mother liquor is crossed the decolouring of D941 decolorizing resin, crosses the AB-8 absorption with macroporous adsorbent resin behind the dilute with water, and ethanol elution detects less than ginsenoside Re and ginsenoside Rg to elutriant
1, reclaim ethanol, get panaxsaponin mixture C 140.3 grams.Detect through HPLC, contain the ginsenoside Rg
122.71%, the ginsenoside Re 9.68%.
Panaxsaponin mixture B 30 grams are crossed neutral alumina post (500 gram) with 400 ml water ultrasonic dissolutions, and first water washes to elutriant and detects less than ginseng saponin F
1Till, elutriant detects less than ginseng saponin F to elutriant with 85% ethanol elution after using the D101 absorption with macroporous adsorbent resin
1, reclaim ethanol, get panaxsaponin mixture D 10.2 grams.Detect through HPLC, contain ginseng saponin F
117.5%, the ginsenoside Rg
23.43%.Wash to elutriant with 50% ethanolic soln then and detect less than ginseng saponin F
2Till N-Fe, elutriant directly reclaims solvent, gets panaxsaponin mixture E 6.3 grams.Detect through HPLC, contain ginseng saponin F
229.53%, N-Fe 6.25%, and the Ginsenoside Rd 17.62%.Be eluted in the elutriant with the aqueous solution of 50% tetrahydrofuran (THF) at last and detect less than Ginsenoside Rd and ginsenoside Rb
1, elutriant reclaims solvent, gets panaxsaponin mixture F 3.4 grams.Detect through HPLC, contain Ginsenoside Rd 22.5%, ginsenoside Rb
211.2%, Ginsenoside Rc 9.5%, ginsenoside Rb
15.8% and ginsenoside Rb
32.2%.
The HPLC condition determination of ginsenoside is as follows: 1. ginsenoside Rg
1, ginsenoside Re's condition determination: chromatographic column: ZORBAX 250 * 4.6mm ODS post; Moving phase: acetonitrile: water=20: 80; Flow velocity: 1.5ml/min; Column temperature: 25 ℃; Detect wavelength: 203nm, below identical; 2. ginsenoside Rb
1, ginsenoside Rb
2, ginsenoside Rb
3, Ginsenoside Rc, Ginsenoside Rd's condition determination: chromatographic column: ZORBAX 250 * 4.6mm ODS post; Moving phase: acetonitrile: water=31: 69; Flow velocity: 1.5ml/min; Column temperature: 25 ℃; Detect wavelength: 203nm, below identical; 3. ginseng saponin F
1, ginseng saponin F
2, the N-Fe condition determination: chromatographic column: ZORBAX 250 * 4.6mm ODS post; Moving phase: acetonitrile: water=38: 62; Flow velocity: 1.5ml/min; Column temperature: 25 ℃; Detect wavelength: 203nm, below identical.
Embodiment 2
7 kilograms of Ginseng Leafs, boiling is extracted three times, each amount of water is respectively 16,14,12 times of Ginseng Leaf's weight, decocting time is respectively 2,1.5,1 hours, merge decoction liquor, cross the D101 absorption with macroporous adsorbent resin, water washes down, and 22% methanol-eluted fractions detects less than ginsenoside Re and ginsenoside Rg to elutriant
1, use 85% ethanol elution then instead and to elutriant, detect less than Ginsenoside Rd and ginsenoside Rb
1Till, collect elutriant respectively.Again cross the AB-8 absorption with macroporous adsorbent resin behind the 22% meoh eluate dilute with water, detect less than ginsenoside Re and ginsenoside Rg to elutriant with 85% ethanol elution then
1, elutriant reclaims ethanol, gets panaxsaponin mixture A 278 grams.Detect through HPLC, contain the ginsenoside Rg
113.36%, the ginsenoside Re 29.68%.85% ethanol eluate directly reclaims ethanol, obtains panaxsaponin mixture B 318 grams.Detect through HPLC, contain ginsenoside Rb
11.73%, ginsenoside Rb
23.69%, ginsenoside Rb
30.58%, Ginsenoside Rc 2.88%, Ginsenoside Rd 7.95%, ginsenoside Rg
10.15%, ginsenoside Re 0.6%, ginseng saponin F
16.15%, ginsenoside Rg
20.8%, ginseng saponin F
25.36%, N-Fe 1.52%.
Panaxsaponin mixture A 270 grams add 540 ml water heating for dissolving, place, and precipitation is filtered, water washing and precipitating, and drying, recrystallization gets ginsenoside Re's 85 grams once more.Detect through HPLC, contain the ginsenoside Rg
11.8%, the ginsenoside Re 98.9%.Mother liquor is crossed the decolouring of D941 decolorizing resin, crosses the D4020 absorption with macroporous adsorbent resin behind the dilute with water, and ethanol elution detects less than ginsenoside Re and ginsenoside Rg to elutriant
1, reclaim ethanol, get panaxsaponin mixture C 131.2 grams.Detect through HPLC, contain the ginsenoside Rg
123.8%, the ginsenoside Re 10.9%.
Panaxsaponin mixture B 100 grams are crossed neutral alumina post (1500 gram) with 1000 ml water ultrasonic dissolutions, and first water washes to elutriant and detects less than ginseng saponin F
1, elutriant detects less than ginseng saponin F to elutriant with 85% ethanol elution after using the AB-8 absorption with macroporous adsorbent resin
1, elutriant reclaims ethanol, reclaims ethanol, gets panaxsaponin mixture D 29 grams.Detect through HPLC, contain ginseng saponin F
116.3%, ginsenoside Rg
23.13%.Wash to elutriant with 55% methanol solution then and detect less than ginseng saponin F
2Till N-Fe, elutriant reclaims solvent, gets panaxsaponin mixture E 25 grams.Detect through HPLC, contain ginseng saponin F
228.33%, N-Fe 9.25%, and the Ginsenoside Rd 11.4%.Be eluted in the elutriant with the aqueous solution of 50% tetrahydrofuran (THF) at last and detect less than Ginsenoside Rd and ginsenoside Rb
1, elutriant reclaims solvent, gets panaxsaponin mixture F 15 grams.Detect through HPLC, contain Ginsenoside Rd 25.0%, ginsenoside Rb
28.8%, Ginsenoside Rc 5.8%, ginsenoside Rb
15.2% and ginsenoside Rb
31.8%.
Embodiment 3
7 kilograms of Ginseng Leafs, boiling is extracted three times, each amount of water is respectively 18,12,8 times of Ginseng Leaf's weight, decocting time is respectively 2,1.5,1 hours, merge decoction liquor, cross the HP-20 absorption with macroporous adsorbent resin, water washes down, and 19% acetone is eluted in the elutriant and detects less than ginsenoside Re and ginsenoside Rg
1, use 85% ethanol elution then instead and to elutriant, detect less than Ginsenoside Rd and ginsenoside Rb
1Till (the TLC method, propyl carbinol: ethyl acetate: water=4: 1: 5, the upper strata, 10% sulfuric acid spraying, 105 ℃ of heating colour developings, below identical), collect elutriant respectively.Again cross the AB-8 absorption with macroporous adsorbent resin behind the 19% acetone elutriant dilute with water, detect less than ginsenoside Re and ginsenoside Rg to elutriant with 85% ethanol elution then
1, elutriant reclaims ethanol, gets panaxsaponin mixture A 287 grams.Detect through HPLC, contain the ginsenoside Rg
113.06%, the ginsenoside Re 29.61%.85% ethanol eluate directly reclaims ethanol, obtains panaxsaponin mixture B 413 grams.Detect through HPLC, contain ginsenoside Rb
11.62%, ginsenoside Rb
23.08%, ginsenoside Rb
30.68%, Ginsenoside Rc 2.91%, Ginsenoside Rd 9.33%, ginsenoside Rg
11.15%, ginsenoside Re 1.06%, ginseng saponin F
16.97%, F
29.19%, N-Fe 3.78%.
Panaxsaponin mixture A 240 grams add 480 milliliter of 10% alcoholic acid aqueous solution heating for dissolving, place, and precipitation is filtered, water washing and precipitating, and drying gets ginsenoside Re's 83 grams.Detect through HPLC, contain the ginsenoside Rg
12.54%, the ginsenoside Re 97.35%.Mother liquor is crossed the decolouring of D941 decolorizing resin, crosses the AB-8 absorption with macroporous adsorbent resin behind the dilute with water, and ethanol elution detects less than ginsenoside Re and ginsenoside Rg to elutriant
1, reclaim ethanol, get panaxsaponin mixture C 120 grams.Detect through HPLC, contain the ginsenoside Rg
135.56%, the ginsenoside Re 13.27%.
Panaxsaponin mixture B 150 gram is crossed neutral alumina post (3000 gram) with 1500 ml water ultrasonic dissolutions, washes to the elutriant detection less than ginseng saponin F with 20% aqueous ethanolic solution earlier
1Till, elutriant detects less than ginseng saponin F to elutriant with 85% ethanol elution after using the AB-8 absorption with macroporous adsorbent resin
1, reclaim ethanol, get panaxsaponin mixture D 35.3 grams.Detect through HPLC, contain ginseng saponin F
116.3%, ginsenoside Rg
23.93%.Wash to elutriant with 65% acetone soln then and detect less than ginseng saponin F
2Till N-Fe, elutriant directly reclaims solvent, gets panaxsaponin mixture E 41.3 grams.Detect through HPLC, contain the ginsenoside Rg
10.20%, ginsenoside Re 0.34%, ginseng saponin F
10.86%, ginseng saponin F
220.53%, N-Fe 5.98%, and the Ginsenoside Rd 12.1%.Be eluted in the elutriant with the aqueous solution of 50% tetrahydrofuran (THF) at last and detect less than Ginsenoside Rd and ginsenoside Rb
1, elutriant reclaims solvent, gets panaxsaponin mixture F 22 grams.Detect through HPLC, contain Ginsenoside Rd 20.8%, ginsenoside Rb
211.9%, Ginsenoside Rc 7.8%, ginsenoside Rb
16.1% and ginsenoside Rb
32.3%.
Embodiment 4
7 kilograms of Ginseng Leafs, boiling is extracted three times, each amount of water is respectively 18,12,8 times of Ginseng Leaf's weight, decocting time is respectively 2,1.5,1 hours, merge decoction liquor, cross 860021 absorption with macroporous adsorbent resin, water washes down, and 20% n-propyl alcohol is eluted in the elutriant and detects less than ginsenoside Re and ginsenoside Rg
1, use 85% ethanol elution then instead and to elutriant, detect less than Ginsenoside Rd and ginsenoside Rb
1Till, collect elutriant respectively.Again cross the AB-8 absorption with macroporous adsorbent resin behind the 20% n-propyl alcohol elutriant dilute with water, detect less than ginsenoside Re and ginsenoside Rg to elutriant with 85% ethanol elution then
1, elutriant reclaims ethanol, gets panaxsaponin mixture A 287 grams.Detect through HPLC, contain the ginsenoside Rg
113.6%, the ginsenoside Re 28.6%.85% ethanol eluate directly reclaims ethanol, obtains panaxsaponin mixture B 413 grams.Detect through HPLC, contain ginsenoside Rb
11.62%, ginsenoside Rb
23.08%, ginsenoside Rb
30.68%, Ginsenoside Rc 2.91%, Ginsenoside Rd 9.33%, ginseng saponin F
16.47%, F
25.12%, N-Fe 2.08%.
Panaxsaponin mixture A 240 grams add 480 milliliter 40% alcoholic acid aqueous solution heating for dissolving, place, and precipitation is filtered, water washing and precipitating, and drying gets ginsenoside Re's 83 grams, detects through HPLC, contains the ginsenoside Rg
11.34%, the ginsenoside Re 97.05%.Mother liquor is crossed the decolouring of D941 decolorizing resin, crosses the AB-8 absorption with macroporous adsorbent resin behind the dilute with water, and ethanol elution detects less than ginsenoside Re and ginsenoside Rg to elutriant
1, reclaim ethanol, get panaxsaponin mixture C 120 grams.Detect through HPLC, contain the ginsenoside Rg
132.26%, the ginsenoside Re 11.07%.
Panaxsaponin mixture B 150 gram is crossed neutral alumina post (3000 gram) with 1500 ml water ultrasonic dissolutions, washes to the elutriant detection less than ginseng saponin F with 15% methanol aqueous solution earlier
1Till, elutriant detects less than ginseng saponin F to elutriant with 85% ethanol elution after using the AB-8 absorption with macroporous adsorbent resin
1, reclaim ethanol, get panaxsaponin mixture D 31.0 grams.Detect through HPLC, contain ginseng saponin F
118.3%, ginsenoside Rg
24.12%.Wash to elutriant with 65% n-propyl alcohol solution then and detect less than ginseng saponin F
2Till N-Fe, elutriant directly reclaims solvent, gets panaxsaponin mixture E 40.3 grams.Detect through HPLC, contain the ginsenoside Rg
10.22%, ginsenoside Re 0.39%, ginseng saponin F
10.96%, ginseng saponin F
220.28%, N-Fe 5.08%, and the Ginsenoside Rd 11.6%.Be eluted in the elutriant with the aqueous solution of 50% tetrahydrofuran (THF) at last and detect less than Ginsenoside Rd and ginsenoside Rb
1, elutriant reclaims solvent, gets panaxsaponin mixture F 21.8 grams.Detect through HPLC, contain Ginsenoside Rd 21.8%, ginsenoside Rb
210.9%, Ginsenoside Rc 7.5%, ginsenoside Rb
16.5% and ginsenoside Rb
32.4%.
Embodiment 5
7 kilograms of Ginseng Leafs, boiling is extracted three times, each amount of water is respectively 18,12,8 times of Ginseng Leaf's weight, decocting time is respectively 2,1.5,1 hours, merge decoction liquor, cross the D201 absorption with macroporous adsorbent resin, water washes down, and 16% Virahol is eluted in the elutriant and detects less than ginsenoside Re and ginsenoside Rg
1, use 85% ethanol elution then instead and to elutriant, detect less than Ginsenoside Rd and ginsenoside Rb
1Till, collect elutriant respectively.16% Virahol elutriant is crossed the AB-8 absorption with macroporous adsorbent resin again, detects less than ginsenoside Re and ginsenoside Rg to elutriant with 85% ethanol elution then
1, elutriant reclaims ethanol, gets panaxsaponin mixture A 297 grams.Detect through HPLC, contain the ginsenoside Rg
113.06%, the ginsenoside Re 29.61%.85% ethanol eluate directly reclaims ethanol, obtains panaxsaponin mixture B 413 grams.Detect through HPLC, contain ginsenoside Rb
11.62%, ginsenoside Rb
23.08%, ginsenoside Rb
30.68%, Ginsenoside Rc 2.91%, Ginsenoside Rd 9.33%, ginseng saponin F
16.97%, F
25.19%, N-Fe 1.78%.
Panaxsaponin mixture A 330 grams add 660 ml water heating for dissolving, place, and precipitation is filtered, water washing and precipitating, and drying gets ginsenoside Re's 99 grams.Detect through HPLC, contain the ginsenoside Rg
11.04%, the ginsenoside Re 97.35%.Mother liquor is crossed the decolouring of D941 decolorizing resin, crosses the AB-8 absorption with macroporous adsorbent resin behind the dilute with water, and ethanol elution detects less than ginsenoside Re and ginsenoside Rg to elutriant
1, reclaim ethanol, get panaxsaponin mixture C150 gram, detect through HPLC, contain the ginsenoside Rg
135.56%, the ginsenoside Re 13.27%.
Panaxsaponin mixture B 150 gram is crossed neutral alumina post (3000 gram) with 1500 ml water ultrasonic dissolutions, washes to the elutriant detection less than ginseng saponin F with 10% aqueous acetone solution earlier
1Till, elutriant detects less than ginseng saponin F to elutriant with 85% ethanol elution after using the AB-8 absorption with macroporous adsorbent resin
1, reclaim ethanol, get panaxsaponin mixture D 34.9 grams.Detect through HPLC, contain ginseng saponin F
119.3%, ginsenoside Rg
23.68%.Wash to elutriant with 55% aqueous isopropanol then and detect less than ginseng saponin F
2Till N-Fe, elutriant directly reclaims solvent, gets panaxsaponin mixture E 42.5 grams.Detect through HPLC, contain the ginsenoside Rg
10.29%, ginsenoside Re 0.24%, ginseng saponin F
10.16%, ginseng saponin F
221.58%, N-Fe 5.28%, and the Ginsenoside Rd 14.10%.Be eluted in the elutriant with the aqueous solution of 50% tetrahydrofuran (THF) at last and detect less than Ginsenoside Rd and ginsenoside Rb
1, elutriant reclaims solvent, gets panaxsaponin mixture F 27.4 grams.Detect through HPLC, contain Ginsenoside Rd 20.1%, ginsenoside Rb
211.3%, Ginsenoside Rc 7.2%, ginsenoside Rb
13.1% and ginsenoside Rb
32.8%.
Embodiment 6
Panaxsaponin mixture B 30 grams are crossed neutral alumina post (600 gram) with 300 ml water ultrasonic dissolutions, and the ethanolic soln with 65% washes to elutriant and detects less than ginseng saponin F
1, ginseng saponin F
2, till the N-Fe, elutriant directly reclaims solvent, panaxsaponin mixture G 15.5 grams.Detect through HPLC, contain ginseng saponin F
112.30%, ginseng saponin F
210.08%, N-Fe 2.05%, Ginsenoside Rd 8.3%.Be eluted in the elutriant with the aqueous solution of 80% tetrahydrofuran (THF) then and detect less than Ginsenoside Rd and ginsenoside Rb
1, elutriant reclaims solvent, gets panaxsaponin mixture F12.0 gram.Detect through HPLC, contain Ginsenoside Rd 20.8%, ginsenoside Rb
211.9%, Ginsenoside Rc 7.8%, ginsenoside Rb
16.1% and ginsenoside Rb
32.3%.
Embodiment 7
Panaxsaponin mixture B 30 grams are crossed neutral alumina post (600 gram) with 300 ml water ultrasonic dissolutions, and the methanol solution with 75% washes to elutriant and detects less than ginseng saponin F
1, ginseng saponin F
2, till the N-Fe, elutriant directly reclaims solvent and gets panaxsaponin mixture G15.5 gram.Detect through HPLC, contain ginseng saponin F
112.30%, ginseng saponin F
212.08%, N-Fe 3.05%, Ginsenoside Rd 6.4%.Be eluted in the elutriant with the aqueous solution of 50% tetrahydrofuran (THF) then and detect less than Ginsenoside Rd and ginsenoside Rb
1, elutriant reclaims solvent, gets panaxsaponin mixture F22 gram.Detect through HPLC, contain Ginsenoside Rd 20.8%, ginsenoside Rb
211.9%, Ginsenoside Rc 7.8%, ginsenoside Rb
16.1% and ginsenoside Rb
32.3%.
Embodiment 8
Panaxsaponin mixture B30 gram is crossed neutral alumina post (600 gram) with 300 ml water ultrasonic dissolutions, and the acetone soln with 75% washes to elutriant and detects less than ginseng saponin F
1, ginseng saponin F
2, till the N-Fe, elutriant directly reclaims solvent, panaxsaponin mixture G15.5 gram.Detect through HPLC, contain ginseng saponin F
112.30%, ginseng saponin F
212.08%, N-Fe 3.05%, Ginsenoside Rd 7.5%.Be eluted in the elutriant with the aqueous solution of 45% tetrahydrofuran (THF) then and detect less than Ginsenoside Rd and ginsenoside Rb
1, elutriant reclaims solvent and gets panaxsaponin mixture F22 gram.Detect through HPLC, contain Ginsenoside Rd 20.8%, ginsenoside Rb
211.9%, Ginsenoside Rc 7.8%, ginsenoside Rb
16.1% and ginsenoside Rb
32.3%.
Embodiment 9
Panaxsaponin mixture B 30 grams are crossed neutral alumina post (600 gram) with 300 ml water ultrasonic dissolutions, and the n-propyl alcohol solution with 75% washes to elutriant and detects less than ginseng saponin F
1, ginseng saponin F
2, till the N-Fe, elutriant directly reclaims solvent, panaxsaponin mixture G15.5 gram.Detect through HPLC, contain ginseng saponin F
112.30%, ginseng saponin F
212.08%, N-Fe 3.05%, Ginsenoside Rd 8.1%.Be eluted in the elutriant with the aqueous solution of 50% tetrahydrofuran (THF) then and detect less than Ginsenoside Rd and ginsenoside Rb
1, elutriant reclaims solvent, gets panaxsaponin mixture F22 gram.Detect through HPLC, contain Ginsenoside Rd 20.8%, ginsenoside Rb
211.9%, Ginsenoside Rc 7.8%, ginsenoside Rb
16.1% and ginsenoside Rb
32.3%.
Embodiment 10
Panaxsaponin mixture B30 gram is crossed neutral alumina post (600 gram) with 300 ml water ultrasonic dissolutions, and the aqueous isopropanol with 75% washes to elutriant and detects less than ginseng saponin F
1, ginseng saponin F
2, till the N-Fe, elutriant directly reclaims solvent, panaxsaponin mixture G15.5 gram.Detect through HPLC, contain ginseng saponin F
112.30%, ginseng saponin F
212.08%, N-Fe 3.05%, Ginsenoside Rd 6.8%.Be eluted in the elutriant with the aqueous solution of 50% tetrahydrofuran (THF) then and detect less than Ginsenoside Rd and ginsenoside Rb
1, elutriant reclaims solvent, gets panaxsaponin mixture F22 gram.Detect through HPLC, contain Ginsenoside Rd 20.8%, ginsenoside Rb
211.9%, Ginsenoside Rc 7.8%, ginsenoside Rb
16.1% and ginsenoside Rb
32.3%.
The present invention utilizes organic solvents such as macroporous adsorbent resin and ethanol with the ginsenoside Rg
1, the ginsenoside Re with other ginsenosides separately, especially with the ginsenoside Rg
1And ginseng saponin F
2, ginsenoside Re and N-Fe separate, thereby obtain only to contain the ginsenoside Rg
1With ginsenoside Re's panaxsaponin mixture with do not contain the ginsenoside Rg
1With ginsenoside Re's panaxsaponin mixture, obtained the efficient part that other means are difficult to obtain.Utilize the method for recrystallization or alumina column chromatography on this basis again, further they are divided into several new panaxsaponin mixtures, and these panaxsaponin mixtures may have different biological activitys or strong biological activity more.Method of the present invention has method uniqueness, simple to operate, remarkable advantage that production cost is low.
Claims (13)
1, a kind of from the Ginseng Leaf extraction separation mainly by ginsenoside Re and ginsenoside Rg
1Composition and ginsenoside Re's content is greater than the ginsenoside Rg
1Panaxsaponin mixture's method, it is characterized in that with extract of Radix Ginseng leaf with absorption with macroporous adsorbent resin after with the aqueous solution wash-out of lower concentration organic solvent.
2, a kind of from the Ginseng Leaf extraction separation mainly by ginsenoside Re and ginsenoside Rg
1Form and the ginsenoside Rg
1Content greater than ginsenoside Re's panaxsaponin mixture's method, it is characterized in that with extract of Radix Ginseng leaf with absorption with macroporous adsorbent resin after with the aqueous solution wash-out of lower concentration organic solvent, the aqueous solution recrystallization of panaxsaponin mixture's water that obtains or alcohol, filter, mother liquor reclaims solvent promptly.
3, a kind of from the Ginseng Leaf extraction separation mainly by ginseng saponin F
1, the ginsenoside Rg
2, ginseng saponin F
2, N-Fe, Ginsenoside Rd, ginsenoside Rb
2, Ginsenoside Rc, ginsenoside Rb
1With ginsenoside Rb
3The panaxsaponin mixture's who forms method is characterized in that the extract of Radix Ginseng leaf absorption with macroporous adsorbent resin, and the aqueous solution of using the lower concentration organic solvent is with the ginsenoside Rg
1With the aqueous solution wash-out of the complete back of ginsenoside Re's wash-out with high levels of organic solvents.
4, a kind of from the Ginseng Leaf extraction separation mainly by ginseng saponin F
1And ginsenoside Rg
2The panaxsaponin mixture's who forms method is characterized in that the extract of Radix Ginseng leaf absorption with macroporous adsorbent resin, and the aqueous solution of using the lower concentration organic solvent is with the ginsenoside Rg
1With the aqueous solution wash-out of the complete back of ginsenoside Re's wash-out with high levels of organic solvents, the panaxsaponin mixture of acquisition goes up alumina column, water wash-out.
5, a kind of from the Ginseng Leaf extraction separation mainly by ginseng saponin F
2, the panaxsaponin mixture that forms of N-Fe, Ginsenoside Rd method, it is characterized in that with the extract of Radix Ginseng leaf absorption with macroporous adsorbent resin aqueous solution of usefulness lower concentration organic solvent is with the ginsenoside Rg
1With the aqueous solution wash-out of the complete back of ginsenoside Re's wash-out with high levels of organic solvents, the panaxsaponin mixture of acquisition goes up alumina column, and water is with ginseng saponin F
1The complete back of the wash-out aqueous solution wash-out of organic solvent.
6, a kind of from the Ginseng Leaf extraction separation mainly by ginseng saponin F
1, the ginsenoside Rg
2, ginseng saponin F
2, the panaxsaponin mixture that forms of N-Fe, Ginsenoside Rd method, it is characterized in that with the extract of Radix Ginseng leaf absorption with macroporous adsorbent resin aqueous solution of usefulness lower concentration organic solvent is with the ginsenoside Rg
1With the aqueous solution wash-out of the complete back of ginsenoside Re's wash-out with high levels of organic solvents, the panaxsaponin mixture of acquisition goes up alumina column, with the aqueous solution wash-out of organic solvent.
7, a kind of from the Ginseng Leaf extraction separation mainly by Ginsenoside Rd, ginsenoside Rb
2, Ginsenoside Rc, ginsenoside Rb
1With ginsenoside Rb
3The panaxsaponin mixture's who forms method is characterized in that the extract of Radix Ginseng leaf absorption with macroporous adsorbent resin, and the aqueous solution of using the lower concentration organic solvent is with the ginsenoside Rg
1With the aqueous solution wash-out of the complete back of ginsenoside Re's wash-out with high levels of organic solvents, the panaxsaponin mixture of acquisition goes up alumina column, and the aqueous solution of using organic solvent is with ginseng saponin F
1, ginseng saponin F
2, the N-Fe wash-out fully the back with the aqueous solution wash-out of tetrahydrofuran (THF).
8, the described preparation method of claim 1 to 7 is characterized in that described macroporous adsorbent resin is selected from one or more of AB-8, D4020,860021, D101, D102, D103, HP20.
9, the described preparation method of claim 1 to 7 is characterized in that described organic solvent is selected from ethanol, methyl alcohol, acetone, n-propyl alcohol, Virahol or their two or more mixture.
10, the described preparation method of claim 1 to 7, the aqueous solution that it is characterized in that described lower concentration organic solvent is concentration of volume percent less than 40% solution.
11, the described preparation method of claim 1 to 7, the aqueous solution that it is characterized in that described high levels of organic solvents is concentration of volume percent greater than 45% solution.
12, the described preparation method of claim 4 to 7 is characterized in that described aluminum oxide is a neutral alumina.
13, the application of panaxsaponin mixture in pharmaceutical compositions, protective foods and ginsenoside monomer of the described preparation method's acquisition of claim 1 to 7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610093612 CN1869056B (en) | 2006-06-21 | 2006-06-21 | Method of extracting and separating ginseng saponine mixture from ginseng leaf |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610093612 CN1869056B (en) | 2006-06-21 | 2006-06-21 | Method of extracting and separating ginseng saponine mixture from ginseng leaf |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1869056A true CN1869056A (en) | 2006-11-29 |
| CN1869056B CN1869056B (en) | 2013-03-20 |
Family
ID=37442851
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200610093612 Expired - Fee Related CN1869056B (en) | 2006-06-21 | 2006-06-21 | Method of extracting and separating ginseng saponine mixture from ginseng leaf |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1869056B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101966220A (en) * | 2009-07-27 | 2011-02-09 | 天津天士力制药股份有限公司 | Panaxtrial saponin extract and preparation process thereof |
| CN101966215A (en) * | 2009-07-27 | 2011-02-09 | 天津天士力制药股份有限公司 | Extracts of panaxtriol saponins and preparation process thereof |
| CN103520014A (en) * | 2012-07-05 | 2014-01-22 | 株式会社爱茉莉太平洋 | Composition for topical skin application containing ginsenoside F2 derived from hydroponic ginseng |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100443086C (en) * | 2004-02-06 | 2008-12-17 | 徐琲琲 | New use of ginseng saponin-Re medicine and its preparation method |
-
2006
- 2006-06-21 CN CN 200610093612 patent/CN1869056B/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101966220A (en) * | 2009-07-27 | 2011-02-09 | 天津天士力制药股份有限公司 | Panaxtrial saponin extract and preparation process thereof |
| CN101966215A (en) * | 2009-07-27 | 2011-02-09 | 天津天士力制药股份有限公司 | Extracts of panaxtriol saponins and preparation process thereof |
| CN103520014A (en) * | 2012-07-05 | 2014-01-22 | 株式会社爱茉莉太平洋 | Composition for topical skin application containing ginsenoside F2 derived from hydroponic ginseng |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1869056B (en) | 2013-03-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1307192C (en) | Process of preparing high-purity jasminodin with Cape jasmine fruit | |
| CN102423329B (en) | A kind of discoloration method of panax notoginsenoside extract | |
| CN102258588A (en) | Preparation method of peony general glycoside | |
| CN1869055A (en) | Method of extracting and separating ginseng saponine monomer from ginseng leaf | |
| CN1869048B (en) | Method of extracting and separating F group ginseng saponin from ginseng leaf | |
| CN109053821A (en) | The method of tea polyphenols, total amino acid, chromocor compound is extracted from grosvenor momordica leaf | |
| CN103180334B (en) | Prepare the method for lactone glucoside of Radix Paeoniae and peoniflorin | |
| CN1869056A (en) | Method of extracting and separating ginseng saponine mixture from ginseng leaf | |
| CN103421058B (en) | A kind of method of high-level efficiency clean cut separation purifying Rhapontin, deoxy- | |
| CN1869051B (en) | Preparation method of trialcohol group ginseng saponine and dialcohol group ginseng saponine | |
| CN102920727B (en) | Method for preparing extracts rich in vitexin rhamnoside and vitexin glucoside | |
| CN105175426A (en) | Method of extracting and purifying bergenin from cissus pteroclada hayata | |
| CN109912582A (en) | The method of mangiferin is extracted from mango leaf | |
| CN112851621B (en) | Total iridoid extract of caulis et folium fici Tikouae, extraction and purification method and application thereof | |
| CN1869058B (en) | Method of preparing trialcohol group ginseng saponine and bialcohol group ginseng saponine from notoginseng | |
| CN100582119C (en) | Process for separating diol ginsenoside and triol ginsenoside | |
| CN1869050B (en) | Method of preparing notoginseng saponine Fe and diol group ginseng saponine from netoginseng leaf | |
| CN1869059B (en) | Method of preparing ginseng saponine monomer from ginseng leaf | |
| CN1869057B (en) | Preparation method of trialcohol group ginseng saponine and bialcohol group ginseng saponine | |
| CN1869053B (en) | Method of extracting and separating ginseng saponine mixture from American ginseng leaf | |
| CN1869052B (en) | Method of extracting and separating ginseng saponine mixture from ginseng leaf | |
| CN101085794B (en) | Method for preparing 10-deacetyl asperulosidic acid methyl ester | |
| CN104987354A (en) | Method for preparing morroniside | |
| CN114907420B (en) | Method for preparing panaxadiol saponins by using polar resin | |
| CN114456138B (en) | Method for separating three coumarin compounds from fingered citron extract |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee |
Owner name: HAINAN ASIAPHARM CO., LTD. Free format text: FORMER NAME: ASIA PHARMACY CO LTD, HAINAN |
|
| CP01 | Change in the name or title of a patent holder |
Address after: Room 1206, commercial building, No. 38 Datong Road, Hainan, Haikou, 570000 Patentee after: Hainan Asia Pharmaceutical Co., Ltd. Address before: Room 1206, commercial building, No. 38 Datong Road, Hainan, Haikou, 570000 Patentee before: Asia Pharmacy Co., Ltd., Hainan |
|
| CP01 | Change in the name or title of a patent holder | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130320 Termination date: 20210621 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |