CN1869056B - 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
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- CN1869056B CN1869056B CN 200610093612 CN200610093612A CN1869056B CN 1869056 B CN1869056 B CN 1869056B CN 200610093612 CN200610093612 CN 200610093612 CN 200610093612 A CN200610093612 A CN 200610093612A CN 1869056 B CN1869056 B CN 1869056B
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Abstract
The present invention discloses a method for extracting and separating ginsenoside mixture from ginseng leaf, especially discloses a method for extracting and separating ginsenoside mixture containing ginsenoside F1, ginsenoside F2 and ginsenoside F3. The method comprises the following steps: adsorbing the ginseng leaf extractive using macroreticular resin; eluting with high-concentration organic solvents after completely eluting ginsenoside Fg1 and eluting ginsenoside Re with low-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 extract the mixture that separates various ginsenoside composition 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 ginseng (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 that is comprised 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, the 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 that forms.
The present invention will provide a kind of novel method of separating various panaxsaponin mixture of extracting from the Ginseng Leaf, especially contain ginseng saponin F
1, ginseng saponin F
2And the panaxsaponin mixture's of N-Fe novel method, be will provide from the Ginseng Leaf, to extract to separate mainly by ginsenoside Re and ginsenoside Rg more specifically
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.
Extract from the Ginseng Leaf at present and separate Ginseng Leaf's total saponins, the most frequently used method is Flavonoids by Macroporous Adsorption Resin.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 aqueous solution of the ethanol of higher concentration, so all saponin(e is eluted, what obtain is Ginseng Leaf's total saponins.We find by research, if transfer the concentration of ethanol lower, namely use the aqueous solution (such as the 18%) wash-out of the ethanol 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 can't detect 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, the upper strata is 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 ginseng saponin F
2, the spot of locating to occur the ginsenoside Re is 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
1Be eluted 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 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 simultaneously a small amount of ginsenoside Rg
2And other people join saponin(e.
There is in the past bibliographical information from the Ginseng Leaf, to separate 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 find that by research Ginseng Leaf's total saponins is 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 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 and extract the mixture that separates the various different ginsenosides that form from the Ginseng Leafs, and namely 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 using first low-concentration ethanol aqueous solution wash-out, at this moment ginsenoside Rg behind the absorption with macroporous adsorbent resin
1Be eluted 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 large Ginsenoside Rds, ginsenoside Rb
2, ginsenoside Rb
1, Ginsenoside Rc, ginsenoside Rb
3Deng still being attracted on the resin.Therefore with the aqueous solution of the ethanol of low concentration with ginsenoside Rg and ginsenoside Re's wash-out fully after, use again the aqueous ethanolic solution wash-out of higher concentration, just can be ginsenoside Re, ginsenoside Rg
1With other ginsenosides separately.
Studies show that further except ethanol, the aqueous solution of the 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, uses first the aqueous solution wash-out of the above-mentioned organic solvent of low concentration, 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, what at this moment elute is to comprise ginseng saponin F again
1, N-Fe and ginseng saponin F
2At other interior ginsenosides, thereby the ginsenoside among the Ginseng Leaf can be divided into two portions, 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 a small amount of residual ginsenoside Re and ginsenoside Rg
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 excessively low, 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 according to the polarity height of macroporous adsorbent resin, select suitable concentration.
Ginsenoside Re and ginsenoside Rg
1Be dissolved in after being eluted 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 again cross macroporous adsorbent resin after adding less dilution, at this moment be dissolved in ginsenoside Re and ginsenoside Rg in the solution
1Will again be attracted on the macroporous adsorbent resin, 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 more simple 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 can obtain respectively ginsenoside Re and mother liquor after the filtration.Mother liquor is crossed absorption with macroporous adsorbent resin again after gac or decolorizing resin decolouring, ethanol elution, and Recycled ethanol, 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 2-3 times of ginsenoside Re, 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
1With ginsenoside Rg2's 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, what at this moment elute is ginseng saponin F again
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 at last the aqueous solution wash-out of tetrahydrofuran (THF), 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 at last the aqueous solution wash-out of tetrahydrofuran (THF), 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 refers to 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 can't detect ginsenoside Re and ginsenoside Rg to elutriant
1After use 85% ethanol elution instead and to elutriant, can't detect Ginsenoside Rd and ginsenoside Rb
1Till (silica gel thin-layer chromatography, propyl carbinol: ethyl acetate: water=4:1:5, the upper strata, 10% sulfate spray, 105 ℃ of heating colour developings, below identical).18% ethanol eluate is crossed the AB-8 absorption with macroporous adsorbent resin again, then can't detect ginsenoside Re and ginsenoside Rg with 85% ethanol elution to elutriant
1, the elutriant Recycled ethanol gets panaxsaponin mixture A308 gram.Detect through HPLC, contain the ginsenoside Rg
19.68%, the ginsenoside Re 22.61%.The direct Recycled ethanol of 85% ethanol eluate obtains panaxsaponin mixture B326 gram.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 A300 gram adds 600 ml water heating for dissolving, places, 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 can't detect ginsenoside Re and ginsenoside Rg to elutriant
1, Recycled ethanol gets panaxsaponin mixture C140.3 gram.Detect through HPLC, contain the ginsenoside Rg
122.71%, the ginsenoside Re 9.68%.
Panaxsaponin mixture B30 gram is crossed neutral alumina column (500 gram) with 400 ml water ultrasonic dissolutions, and first water washes to elutriant and can't detect ginseng saponin F
1Till, elutriant can't detect ginseng saponin F with 85% ethanol elution after with the D101 absorption with macroporous adsorbent resin to elutriant
1, Recycled ethanol gets panaxsaponin mixture D10.2 gram.Detect through HPLC, contain ginseng saponin F
117.5%, the ginsenoside Rg
23.43%.Then wash to elutriant with 50% ethanolic soln and can't detect ginseng saponin F
2Till N-Fe, elutriant directly reclaims solvent, gets panaxsaponin mixture E6.3 gram.Detect through HPLC, contain ginseng saponin F
229.53%, N-Fe 6.25%, and the Ginsenoside Rd 17.62%.Be eluted to the aqueous solution of 50% tetrahydrofuran (THF) at last and can't detect Ginsenoside Rd and ginsenoside Rb in the elutriant
1, elutriant reclaims solvent, gets panaxsaponin mixture F3.4 gram.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: ZORBAX250 * 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: ZORBAX250 * 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: ZORBAX250 * 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 can't detect ginsenoside Re and ginsenoside Rg to elutriant
1, then use 85% ethanol elution instead and to elutriant, can't detect Ginsenoside Rd and ginsenoside Rb
1Till, collect respectively elutriant.Again cross the AB-8 absorption with macroporous adsorbent resin behind the 22% meoh eluate dilute with water, then to elutriant, can't detect ginsenoside Re and ginsenoside Rg with 85% ethanol elution
1, the elutriant Recycled ethanol gets panaxsaponin mixture A278 gram.Detect through HPLC, contain the ginsenoside Rg
113.36%, the ginsenoside Re 29.68%.The direct Recycled ethanol of 85% ethanol eluate obtains panaxsaponin mixture B318 gram.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 A270 gram adds 540 ml water heating for dissolving, places, and precipitation is filtered, water washing and precipitating, and drying, recrystallization gets ginsenoside Re's 85 grams again.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 can't detect ginsenoside Re and ginsenoside Rg to elutriant
1, Recycled ethanol gets panaxsaponin mixture C131.2 gram.Detect through HPLC, contain the ginsenoside Rg
123.8%, the ginsenoside Re 10.9%.
Panaxsaponin mixture B100 gram is crossed neutral alumina column (1500 gram) with 1000 ml water ultrasonic dissolutions, and first water washes to elutriant and can't detect ginseng saponin F
1, elutriant can't detect ginseng saponin F with 85% ethanol elution after with the AB-8 absorption with macroporous adsorbent resin to elutriant
1, the elutriant Recycled ethanol, Recycled ethanol gets panaxsaponin mixture D29 gram.Detect through HPLC, contain ginseng saponin F
116.3%, ginsenoside Rg
23.13%.Then wash to elutriant with 55% methanol solution and can't detect ginseng saponin F
2Till N-Fe, elutriant reclaims solvent, gets panaxsaponin mixture E25 gram.Detect through HPLC, contain ginseng saponin F
228.33%, N-Fe 9.25%, and the Ginsenoside Rd 11.4%.Be eluted to the aqueous solution of 50% tetrahydrofuran (THF) at last and can't detect Ginsenoside Rd and ginsenoside Rb in the elutriant
1, elutriant reclaims solvent, gets panaxsaponin mixture F15 gram.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 to and can't detect ginsenoside Re and ginsenoside Rg in the elutriant
1, then use 85% ethanol elution instead and to elutriant, can't detect Ginsenoside Rd and ginsenoside Rb
1Till (the TLC method, propyl carbinol: ethyl acetate: water=4:1:5, the upper strata, 10% sulfate spray, 105 ℃ of heating colour developings, below identical), collect respectively elutriant.Again cross the AB-8 absorption with macroporous adsorbent resin behind the 19% acetone elutriant dilute with water, then to elutriant, can't detect ginsenoside Re and ginsenoside Rg with 85% ethanol elution
1, the elutriant Recycled ethanol gets panaxsaponin mixture A287 gram.Detect through HPLC, contain the ginsenoside Rg
113.06%, the ginsenoside Re 29.61%.The direct Recycled ethanol of 85% ethanol eluate obtains panaxsaponin mixture B413 gram.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 A240 restrains, and adds the aqueous solution heating for dissolving of 480 milliliter of 10% ethanol, places, 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 can't detect ginsenoside Re and ginsenoside Rg to elutriant
1, Recycled ethanol gets panaxsaponin mixture C120 gram.Detect through HPLC, contain the ginsenoside Rg
135.56%, the ginsenoside Re 13.27%.
Panaxsaponin mixture B150 gram is crossed neutral alumina column (3000 restrain) with 1500 ml water ultrasonic dissolutions, washes to elutriant with 20% aqueous ethanolic solution first and can't detect ginseng saponin F
1Till, elutriant can't detect ginseng saponin F with 85% ethanol elution after with the AB-8 absorption with macroporous adsorbent resin to elutriant
1, Recycled ethanol gets panaxsaponin mixture D35.3 gram.Detect through HPLC, contain ginseng saponin F
116.3%, ginsenoside Rg
23.93%.Then wash to elutriant with 65% acetone soln and can't detect ginseng saponin F
2Till N-Fe, elutriant directly reclaims solvent, gets panaxsaponin mixture E41.3 gram.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 to the aqueous solution of 50% tetrahydrofuran (THF) at last and can't detect Ginsenoside Rd and ginsenoside Rb in the elutriant
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 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 to and can't detect ginsenoside Re and ginsenoside Rg in the elutriant
1, then use 85% ethanol elution instead and to elutriant, can't detect Ginsenoside Rd and ginsenoside Rb
1Till, collect respectively elutriant.Again cross the AB-8 absorption with macroporous adsorbent resin behind the 20% n-propyl alcohol elutriant dilute with water, then to elutriant, can't detect ginsenoside Re and ginsenoside Rg with 85% ethanol elution
1, the elutriant Recycled ethanol gets panaxsaponin mixture A287 gram.Detect through HPLC, contain the ginsenoside Rg
113.6%, the ginsenoside Re 28.6%.The direct Recycled ethanol of 85% ethanol eluate obtains panaxsaponin mixture B413 gram.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 A240 restrains, and adds the aqueous solution heating for dissolving of 480 milliliter 40% ethanol, places, and precipitation is filtered, water washing and precipitating, and drying gets ginsenoside Re's 83 grams, through the HPLC detection, 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 can't detect ginsenoside Re and ginsenoside Rg to elutriant
1, Recycled ethanol gets panaxsaponin mixture C120 gram.Detect through HPLC, contain the ginsenoside Rg
132.26%, the ginsenoside Re 11.07%.
Panaxsaponin mixture B150 gram is crossed neutral alumina column (3000 restrain) with 1500 ml water ultrasonic dissolutions, washes to elutriant with 15% methanol aqueous solution first and can't detect ginseng saponin F
1Till, elutriant can't detect ginseng saponin F with 85% ethanol elution after with the AB-8 absorption with macroporous adsorbent resin to elutriant
1, Recycled ethanol gets panaxsaponin mixture D31.0 gram.Detect through HPLC, contain ginseng saponin F
118.3%, ginsenoside Rg
24.12%.Then wash to elutriant with 65% n-propyl alcohol solution and can't detect ginseng saponin F
2Till N-Fe, elutriant directly reclaims solvent, gets panaxsaponin mixture E40.3 gram.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 to the aqueous solution of 50% tetrahydrofuran (THF) at last and can't detect Ginsenoside Rd and ginsenoside Rb in the elutriant
1, elutriant reclaims solvent, gets panaxsaponin mixture F21.8 gram.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 to and can't detect ginsenoside Re and ginsenoside Rg in the elutriant
1, then use 85% ethanol elution instead and to elutriant, can't detect Ginsenoside Rd and ginsenoside Rb
1Till, collect respectively elutriant.16% Virahol elutriant is crossed the AB-8 absorption with macroporous adsorbent resin again, then can't detect ginsenoside Re and ginsenoside Rg with 85% ethanol elution to elutriant
1, the elutriant Recycled ethanol gets panaxsaponin mixture A297 gram.Detect through HPLC, contain the ginsenoside Rg
113.06%, the ginsenoside Re 29.61%.The direct Recycled ethanol of 85% ethanol eluate obtains panaxsaponin mixture B413 gram.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 A330 gram adds 660 ml water heating for dissolving, places, 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 can't detect ginsenoside Re and ginsenoside Rg to elutriant
1, Recycled ethanol gets panaxsaponin mixture C150 gram, detects through HPLC, contains the ginsenoside Rg
135.56%, the ginsenoside Re 13.27%.
Panaxsaponin mixture B150 gram is crossed neutral alumina column (3000 restrain) with 1500 ml water ultrasonic dissolutions, washes to elutriant with 10% aqueous acetone solution first and can't detect ginseng saponin F
1Till, elutriant can't detect ginseng saponin F with 85% ethanol elution after with the AB-8 absorption with macroporous adsorbent resin to elutriant
1, Recycled ethanol gets panaxsaponin mixture D34.9 gram.Detect through HPLC, contain ginseng saponin F
119.3%, ginsenoside Rg
23.68%.Then wash to elutriant with 55% aqueous isopropanol and can't detect ginseng saponin F
2Till N-Fe, elutriant directly reclaims solvent, gets panaxsaponin mixture E42.5 gram.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 to the aqueous solution of 50% tetrahydrofuran (THF) at last and can't detect Ginsenoside Rd and ginsenoside Rb in the elutriant
1, elutriant reclaims solvent, gets panaxsaponin mixture F27.4 gram.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 B30 gram is crossed neutral alumina column (600 gram) with 300 ml water ultrasonic dissolutions, and the ethanolic soln with 65% washes to elutriant and can't detect ginseng saponin F
1, ginseng saponin F
2, till the N-Fe, elutriant directly reclaims solvent, gets panaxsaponin mixture G15.5 gram.Detect through HPLC, contain ginseng saponin F
112.30%, ginseng saponin F
210.08%, N-Fe 2.05%, Ginsenoside Rd 8.3%.Then be eluted to the aqueous solution of 80% tetrahydrofuran (THF) and can't detect Ginsenoside Rd and ginsenoside Rb in the elutriant
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 B30 gram is crossed neutral alumina column (600 gram) with 300 ml water ultrasonic dissolutions, and the methanol solution with 75% washes to elutriant and can't detect 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%.Then be eluted to the aqueous solution of 50% tetrahydrofuran (THF) and can't detect Ginsenoside Rd and ginsenoside Rb in the elutriant
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 column (600 gram) with 300 ml water ultrasonic dissolutions, and the acetone soln with 75% washes to elutriant and can't detect ginseng saponin F
1, ginseng saponin F
2, till the N-Fe, elutriant directly reclaims solvent, 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 7.5%.Then be eluted to the aqueous solution of 45% tetrahydrofuran (THF) and can't detect Ginsenoside Rd and ginsenoside Rb in the elutriant
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 B30 gram is crossed neutral alumina column (600 gram) with 300 ml water ultrasonic dissolutions, and the n-propyl alcohol solution with 75% washes to elutriant and can't detect ginseng saponin F
1, ginseng saponin F
2, till the N-Fe, elutriant directly reclaims solvent, 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 8.1%.Then be eluted to the aqueous solution of 50% tetrahydrofuran (THF) and can't detect Ginsenoside Rd and ginsenoside Rb in the elutriant
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 column (600 gram) with 300 ml water ultrasonic dissolutions, and the aqueous isopropanol with 75% washes to elutriant and can't detect ginseng saponin F
1, ginseng saponin F
2, till the N-Fe, elutriant directly reclaims solvent, 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 6.8%.Then be eluted to the aqueous solution of 50% tetrahydrofuran (THF) and can't detect Ginsenoside Rd and ginsenoside Rb in the elutriant
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 the 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 again on this basis the method for recrystallization or alumina column chromatography, 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 (6)
1. one kind is extracted separation mainly by ginseng saponin F from the Ginseng Leaf
1, the ginsenoside Rg
2, ginseng saponin F
2, arasaponin F
e, 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, uses the aqueous solution of lower concentration organic solvent with the ginsenoside Rg
1With ginsenoside Re's wash-out fully after with the aqueous solution wash-out of high levels of organic solvents, wherein the aqueous solution of lower concentration organic solvent is concentration expressed in percentage by volume less than 40% solution, the aqueous solution of high levels of organic solvents is concentration expressed in percentage by volume greater than 45% solution; Described organic solvent is selected from ethanol, methyl alcohol, acetone, n-propyl alcohol, Virahol or their two or more mixtures; Described macroporous resin is selected from a kind of of AB-8, D4020,860021, D101, D102, D103, HP20.
2. one kind is extracted separation mainly by ginseng saponin F from the Ginseng Leaf
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, uses the aqueous solution of lower concentration organic solvent with the ginsenoside Rg
1With the fully rear aqueous solution wash-out with high levels of organic solvents of ginsenoside Re's wash-out, the upper alumina column of the panaxsaponin mixture who obtains, wash with water, wherein the aqueous solution of lower concentration organic solvent is concentration expressed in percentage by volume less than 40% solution, and the aqueous solution of high levels of organic solvents is concentration expressed in percentage by volume greater than 45% solution; Described organic solvent is selected from ethanol, methyl alcohol, acetone, n-propyl alcohol, Virahol or their two or more mixtures; Described macroporous resin is selected from a kind of of AB-8, D4020,860021, D101, D102, D103, HP20.
3. one kind is extracted separation mainly by ginseng saponin F from the Ginseng Leaf
2, arasaponin F
e, the panaxsaponin mixture that forms of 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 fully rear aqueous solution wash-out with high levels of organic solvents of ginsenoside Re's wash-out, the upper alumina column of the panaxsaponin mixture of acquisition, water is with ginseng saponin F
1Wash-out fully after with the aqueous solution wash-out of organic solvent, wherein the aqueous solution of lower concentration organic solvent is concentration expressed in percentage by volume less than 40% solution, the aqueous solution of high levels of organic solvents is concentration expressed in percentage by volume greater than 45% solution; Described organic solvent is selected from ethanol, methyl alcohol, acetone, n-propyl alcohol, Virahol or their two or more mixtures; Described macroporous resin is selected from a kind of of AB-8, D4020,860021, D101, D102, D103, HP20.
4. one kind is extracted separation mainly by ginseng saponin F from the Ginseng Leaf
1, the ginsenoside Rg
2, ginseng saponin F
2, arasaponin F
e, the panaxsaponin mixture that forms of 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 fully rear aqueous solution wash-out with high levels of organic solvents of ginsenoside Re's wash-out, the upper alumina column of the panaxsaponin mixture who obtains, aqueous solution wash-out with organic solvent, wherein the aqueous solution of lower concentration organic solvent is concentration expressed in percentage by volume less than 40% solution, and the aqueous solution of high levels of organic solvents is concentration expressed in percentage by volume greater than 45% solution; Described organic solvent is selected from ethanol, methyl alcohol, acetone, n-propyl alcohol, Virahol or their two or more mixtures; Described macroporous resin is selected from a kind of of AB-8, D4020,860021, D101, D102, D103, HP20.
5. one kind is extracted separation mainly by Ginsenoside Rd, ginsenoside Rb from the Ginseng Leaf
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, uses the aqueous solution of lower concentration organic solvent with the ginsenoside Rg
1With the fully rear aqueous solution wash-out with high levels of organic solvents of ginsenoside Re's wash-out, the upper alumina column of the panaxsaponin mixture of acquisition uses the aqueous solution wash-out of organic solvent with ginseng saponin F
1, ginseng saponin F
2, arasaponin F
eWash-out fully after with the aqueous solution wash-out of tetrahydrofuran (THF), wherein the aqueous solution of lower concentration organic solvent is concentration expressed in percentage by volume less than 40% solution, the aqueous solution of high levels of organic solvents is concentration expressed in percentage by volume greater than 45% solution; Described organic solvent is selected from ethanol, methyl alcohol, acetone, n-propyl alcohol, Virahol or their two or more mixtures; Described macroporous resin is selected from a kind of of AB-8, D4020,860021, D101, D102, D103, HP20.
6. such as each described preparation method of claim 2-5, described aluminum oxide is neutral alumina.
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| KR101877801B1 (en) * | 2012-07-05 | 2018-07-13 | (주)아모레퍼시픽 | Composition of skin external application containing ginsenoside F2 derive from hydroponic ginseng |
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| 张崇禧等.大孔树脂吸附人参总皂苷工艺及再生使用的研究.《中国药学杂志》.2003,第38卷(第9期),661-664. * |
| 赵瑜等.大孔吸附树脂分离纯化人参二醇类和三醇类皂甙.《天然产物研究与开发》.2004,第16卷(第3期),235-238. * |
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