CN101224224A - Method for extracting crude flavone and flavone glycoside from ginkgo leafs - Google Patents
Method for extracting crude flavone and flavone glycoside from ginkgo leafs Download PDFInfo
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- CN101224224A CN101224224A CNA2008100100127A CN200810010012A CN101224224A CN 101224224 A CN101224224 A CN 101224224A CN A2008100100127 A CNA2008100100127 A CN A2008100100127A CN 200810010012 A CN200810010012 A CN 200810010012A CN 101224224 A CN101224224 A CN 101224224A
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Abstract
The invention provides a method for extracting crude flavonoids and glycoside from ginkgo leaves, which relates to an extracting method of drug, in particular to an extracting and purifying method of effective components of Chinese medicine. Flocculating clarification method is used for treating water extract of ginkgo leaves; then purification is carried out before alcohol precipitation; chitosan with selective adsorption is taken as a clarifier of the water extract of ginkgo leaves. Flocculation is carried out for removing impurities before adopting the alcohol precipitation method of the water extract of ginkgo leaves to extract crude flavonoids and glycoside; a selective flocculation method is adopted to purify impurities of the water extract of ginkgo leaves. The crude flavonoids and glycoside processed by taking chitosan as clarifier of the invention are bright yellow, have an obviously superior quality to the crude flavonoids and glycoside processed by a traditional method and are suitable for pharmacy.
Description
Technical field
The present invention relates to a kind of extracting method of medical material, particularly relate to a kind of extraction and purification method of middle pharmaceutically active ingredient.
Background technology
The common method of herbal pharmaceutical enterprise Chinese medicine extraction and cleaning is a decoction and alcohol sedimentation technique at present, decoction and alcohol sedimentation technique is solvent with water, to Chinese crude drug decoct, essence carries, be clarifier again with ethanol, the water extract is carried out clarifying treatment, most of polysaccharide in the removal Chinese traditional medicine water extract, protein, resin etc. reclaim ethanol at last, obtain the extract solution of clear.This kind method be applicable to contained effective ingredient to thermally-stabilised, can be water-soluble, and can be dissolved in the alcoholic acid Chinese crude drug of finite concentration.Though use alcohol deposition method can obtain limpid effective ingredient solution, have also that finished product stability is relatively poor, ethanol consumes big, complex process, cost is higher and shortcoming such as serious waste of resources.Again the macromole effective ingredient (as protein and part polysaccharide) of some alcohol insoluble matters in the Chinese medicine is removed as impurity simultaneously at the clarification medicinal liquid, and these compositions particularly polysaccharide show to have enhance immunity effect and physiologically active widely by pharmacology, immunology and clinical research, be difficult to guarantee the less stable of the effectiveness and the finished product of finished product preparation.
Summary of the invention
The object of the present invention is to provide the process of Folium Ginkgo water extract alcohol deposition method is improved, before precipitate with ethanol, use has the clarifier of the chitosan of selective absorption effect as Folium Ginkgo water extract, by flocculence Folium Ginkgo water extract is carried out defecate and purify to remove impurity, reach the purpose of the active constituent content that improves crude flavonoid and flavonoid glycoside.
The objective of the invention is to be achieved through the following technical solutions:
Extract the method for crude flavonoid and flavone glycoside in the Folium Ginkgo, utilize flocculate and clarify method Processing Ag Folium Pruni water extract; Before precipitate with ethanol, purify; Use has the clarifier of the chitosan of selective absorption effect as Folium Ginkgo water extract.
Extract the method for crude flavonoid and flavone glycoside in the described Folium Ginkgo, before Folium Ginkgo water extract alcohol deposition method extracts crude flavonoid and flavone glycoside, use the flocculence remove impurity.
Extract the method for crude flavonoid and flavone glycoside in the described Folium Ginkgo, Folium Ginkgo water extract is used the method purification and impurity removal of selective flocculation.
Advantage of the present invention and effect are:
The present invention obtains as drawing a conclusion by chitosan flocculant being used for the purification and impurity removal of Folium Ginkgo water extract:
1. the clarifier chitosan selected for use of the present invention has good clarification to Folium Ginkgo water extract, and flocculating rate can reach more than 90%.
2. chitosan has selectivity to the flocculation of Folium Ginkgo water extract, and only the impurity in the flocculating sedimentation medicinal liquid does not work to effective ingredient substantially, and the total flavones loss rate is lower than 3%.
3. the Folium Ginkgo water extract general flavone content of flocculence processing is higher by 5.4% than decoction and alcohol sedimentation technique, and is higher by 21% than alcohol extracting method.
4. the crude flavonoid and the flavone glycoside of the clarifier treatment with chitosan selected for use of the present invention are glassy yellow, and quality is more suitable for pharmacy significantly better than resulting crude flavonoid of traditional method and flavone glycoside.
Description of drawings
Fig. 1 is the influence of chitosan addition of the present invention to flocculating effect;
Fig. 2 is the change curve of total flavones loss rate of the present invention with pH value;
Fig. 3 is the relation curve of temperature of the present invention to the influence of total flavones loss rate;
Fig. 4 is the flocculate sketch map of colloid solution when not adding flocculating agent in the principle of the present invention;
Fig. 5 is adsorbed on sketch map on the granule for flocculate flocculating agent in the principle of the present invention;
Fig. 6 adds the sketch map that flocculating agent stirs back colloid solution for the present invention's principle of flocculating;
Fig. 7 is the preceding two kinds of different in kind pimpled rubber liquid solution sketch maps of selective flocculation of the present invention;
Fig. 8 is sketch map behind the colloid solution selective flocculation of the present invention;
The mechanism sketch map that Fig. 9 a builds bridge for flocculate with chitosan effect of the present invention;
Fig. 9 b is a flocculate with chitosan effect charge neutralization sketch map of the present invention;
Fig. 9 c catches volume for flocculate with chitosan effect net of the present invention and sweeps sketch map.
The specific embodiment
The present invention is described in detail with reference to the accompanying drawings.
The alcohol deposition method of the characteristics of Folium Ginkgo water extract and Folium Ginkgo water extract:
The colloidal solid that in Folium Ginkgo water extract, has two kinds of different in kinds, effective ingredient colloid and impurity colloid, wherein the colloidal granularity of effective ingredient is much smaller than the colloidal granularity of impurity.
Alcohol deposition method is the common method of Chinese medicine modern production, and it mainly utilizes impurity such as protein, starch, polysaccharide to be insoluble to alcohol, and middle pharmaceutically active ingredient is dissolved in the character of alcohol and realizes that active ingredient and impurity are isolating.Alcohol deposition method divides two kinds of decoction and alcohol sedimentation technique and alcohol extracting methods.Decoction and alcohol sedimentation technique generally concentrates the back with Chinese traditional medicine water extract and adds alcohol, makes the determining alcohol of medicinal liquid surpass 80%, and the impurity that at this moment is insoluble to alcohol just settles, and effective ingredient is dissolved in the pure liquid, has realized the separation of active ingredient.
Because the impurity colloidal solid is insoluble to alcohol in the Folium Ginkgo water extract, the effective ingredient colloidal solid is dissolved in alcohol, therefore adopts water extract alcohol deposition method to obtain purified crude flavonoid and flavone glycoside.
Flocculate and clarify method principle:
The flocculate and clarify technology is a kind of emerging Chinese medicine production technology, it utilizes in the nontoxic flocculating agent absorption Chinese traditional medicine water extract can not settled small impurity particle, make it to be combined into and bigger can purify Chinese traditional medicine water extract by settled floc sedimentation, shown in Fig. 4,5,6, flocculating agent is adsorbed on the colloidal solid after adding colloid solution, form floc sedimentation and sedimentation through mechanical dehydration (stirring), flocculence is achieved success in some Chinese medicine productions, but also is not applied to the report that Folium Ginkgo is produced.
Be insoluble in the Chinese traditional medicine water extract (effective ingredient the same colloid that is with impurity in the water extract exists) of water for effective ingredient, should use the purpose of the method realization removal impurity of selective flocculation, the principle of selective flocculation is shown in Fig. 7,8, a kind of colloidal solid in the flocculating agent adsorption-flocculation colloid solution (colloidal solid) with two or more different in kinds, and keep the granule of other kind.
Chitosan has the selective flocculation adsorption to Folium Ginkgo water extract:
Chitosan has the selective flocculation adsorption as the clarifier of Folium Ginkgo water extract, it is flocculation absorption impurity colloidal solid only, and the effective ingredient colloidal solid is not produced adsorption, thereby realized flocculating sedimentation impurity optionally and kept the purpose of effective ingredient, for alcohol deposition method extracts more purified crude flavonoid and flavone glycoside provides condition.
Chitosan has the dual function of charging neutrality flocculation and adsorption-flocculation concurrently as flocculating agent: one side makes colloidal solid take off steady by charging neutrality and forms tiny agglomerate; Make these agglomerates form the floc sedimentation of large volume by the macromolecule bridging action on the other hand.
In flocculation Folium Ginkgo water extract process, a large amount of free hydroxyl groups and amino owing to distributing on the chitosan molecule chain, amino is protonated easily in dilute acid soln, thereby make and have a large amount of positive charges on the chitosan molecule chain, become a kind of polyelectrolyte of solubility, have the effect of cationic flocculant.And the impurity particle in the Folium Ginkgo water extract has negative charge, has just constituted the adsorption-flocculation of xenogenesis electric charge.
Chitosan flocculant is to the flocculation of Folium Ginkgo water extract, at first attracted on the particle in the Folium Ginkgo water extract by electrostatic interaction, and between different particles, build bridge, and then formed bigger floc sedimentation by the compression of charging neutrality and electric double layer, in the sinking process of floc sedimentation, constantly roll up the fine particle of sweeping in the water extract, form flocculent deposit at last, reach the purpose of primary water extract.Be depicted as chitosan flocculant three kinds of schematic diagrams of flocculation as Fig. 9 a～9c to Folium Ginkgo water extract.
The preparation of ginkgo biloba succi
Take by weighing Folium Ginkgo medicated powder (filtration of 100 orders) 50g and put into the 1000mL flask, in flask, add 500mL warm water (35 ℃～45 ℃) earlier and soak about 20min, be heated to boiling then, decoct 1h, stop heating, the cooling back is extruded onto filtering residue half-dried with screen cloth (200 order) three layer filtration, put into flask once more, in flask, add 400mL hot water, continue to be heated to boiling, stop heating behind the 1h, cooling, filter, extract medicinal residues, merge filtrate twice, and the way of employing dilution or evaporation and concentration, guarantee that crude drug concentration is 0.1g/mL.
The preparation of chitosan solution
It is 1% chitosan solution that acetic acid solutions with 1% becomes concentration, fully uses immediately as flocculating agent after the swelling, in order to avoid slowly hydrolysis and influence flocculating effect in diluted acid.
The decoction and alcohol sedimentation technique operational approach: get ginkgo biloba succi 50mL heating and concentrate, add an amount of dehydrated alcohol then, make that liquor strength is 0.1g/mL, the limit edged stirs, and removes precipitation after leaving standstill 24h, can obtain purified crude flavonoid and flavonoid glycoside.
Claims (3)
1. extract the method for crude flavonoid and flavone glycoside in the Folium Ginkgo, it is characterized in that: utilize flocculate and clarify method Processing Ag Folium Pruni water extract; Before precipitate with ethanol, purify; Use has the clarifier of the chitosan of selective absorption effect as Folium Ginkgo water extract.
2. extract the method for crude flavonoid and flavone glycoside in the Folium Ginkgo according to claim 1, it is characterized in that before Folium Ginkgo water extract alcohol deposition method extracts crude flavonoid and flavone glycoside, using the flocculence remove impurity.
3. extract the method for crude flavonoid and flavone glycoside in the Folium Ginkgo according to claim 1, it is characterized in that Folium Ginkgo water extract is used the method purification and impurity removal of selective flocculation.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100100127A CN101224224A (en) | 2008-01-02 | 2008-01-02 | Method for extracting crude flavone and flavone glycoside from ginkgo leafs |
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| CNA2008100100127A CN101224224A (en) | 2008-01-02 | 2008-01-02 | Method for extracting crude flavone and flavone glycoside from ginkgo leafs |
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| CNA2008100100127A Pending CN101224224A (en) | 2008-01-02 | 2008-01-02 | Method for extracting crude flavone and flavone glycoside from ginkgo leafs |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104522217A (en) * | 2015-01-22 | 2015-04-22 | 重庆中宝生物制药有限公司 | Vine tea extract and applications thereof |
| CN108676616A (en) * | 2018-05-15 | 2018-10-19 | 王成 | A kind of preparation method of natural tobacco aromaticss |
| CN114470061A (en) * | 2020-10-23 | 2022-05-13 | 昆药集团股份有限公司 | New extraction process of 'Dingyinnaotong' pharmaceutical composition and new applicable crowd thereof |
-
2008
- 2008-01-02 CN CNA2008100100127A patent/CN101224224A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104522217A (en) * | 2015-01-22 | 2015-04-22 | 重庆中宝生物制药有限公司 | Vine tea extract and applications thereof |
| CN108676616A (en) * | 2018-05-15 | 2018-10-19 | 王成 | A kind of preparation method of natural tobacco aromaticss |
| CN114470061A (en) * | 2020-10-23 | 2022-05-13 | 昆药集团股份有限公司 | New extraction process of 'Dingyinnaotong' pharmaceutical composition and new applicable crowd thereof |
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Open date: 20080723 |