CN101343330A - Preparation method for panax ginseng polyoses extract - Google Patents
Preparation method for panax ginseng polyoses extract Download PDFInfo
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- CN101343330A CN101343330A CNA2008100126485A CN200810012648A CN101343330A CN 101343330 A CN101343330 A CN 101343330A CN A2008100126485 A CNA2008100126485 A CN A2008100126485A CN 200810012648 A CN200810012648 A CN 200810012648A CN 101343330 A CN101343330 A CN 101343330A
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Abstract
The invention relates to a preparation method of ginseng polysaccharide extractive. Ginseng coarse powder is adopted, ethanol of 60 percent to 80 percent which occupies eight times to ten times of the amount of ginseng coarse powder is added to perform reflux extraction for two to three times, decoction dregs is filtered to clean out ethanol, the purified water ten times to fifteen times of the decoction dregs is added, then hydrochloric acid is added, the pH value is regulated to be one to three, boiling-out is performed for half to two hours, the decoction dregs is filtered to repeat boiling-out once, the extracted solution is combined, filtered through and decompressed and condensed, to obtain the extracted concentrated solution, hydrochloric acid is added in the extracted concentrated solution, the pH value is regulated to be one to three, hydrogen peroxide four times to six times of the amount of hydrochloric acid is added and is agitated and thermally preserved under the temperature of 85 DEG C to 95 DEG C for one to three hours, the extracted concentrated solution is cooled to the room temperature and filtered, and the concentrated solution after being decolorized is obtained; the pH value of the concentrated solution after being decolorized is regulated by utilizing NaOH to be three to five, ethanol two times to five times the concentrated solution is added, the concentrated solution is evenly agitated and is allowed to stand, precipitation is leached and cleaned for one time by utilizing ethanol with 60 percent to 80 percent containing HCl with 0.2 percent to 2.0 percent, the precipitate is dissolved through water, the alcohol precipitation washing and the acid alcohol washing are respectively repeated for once, and white ginseng polysaccharide extractive is obtained..
Description
Technical field:
The present invention relates to a kind of new extraction process for purification that from the ginseng crude drug, extracts the panaxan, and relate to the preparation method of ginseng polysaccharide injection, powder injection and other medicines preparation, be used for the side effect that ameliorate tumor is put, chemotherapy causes, can be used as the adjuvant drug of immunomodulatory and oncotherapy.
Background technology:
Genseng reinforces vital energy as famous and precious traditional tonic Chinese medicine material, promotes the production of body fluid the effect of calming the nerves admittedly take off.Just be applied to clinically as far back as period in time immemorial, through the analysis of effective component that modern technology is carried out genseng, reference's gracilis polysaccharide is one of pharmacological component main in the genseng.Genseng contains various saccharides (its total sugar content is 4%～6%), comprises monose, oligose and polysaccharide.The panaxan is made up of genseng starch and ginseng pectin's analogue two portions, and the pharmacologically active part mainly is ginseng pectin's analogue.The panaxan who from ginseng, extracts, the 80%th, genseng starch, the ginseng pectin after amylase is sloughed starch mainly is made up of galacturonic acid (GalA), semi-lactosi (Gal), pectinose (Ara) residue, also has a small amount of rhamnosyl (Rha) residue.
Since the eighties, people have carried out deep research to the panaxan.To so far, Chinese scholars has been separated from genseng and has been obtained 30 various human gracilis polysaccharides.Experiment shows that these polysaccharide can strengthen the phagocytic function of reticuloendothelial system, and the generation of complement and antibody in the stimulation blood increases the content of immunoglobulin (Ig) in the blood and can suppress S
180, EAC and U
14Deng the growth of experimental tumor, strengthen the endoxan antitumor action.Therefore, but panaxan's preparation enhancing body immunoloregulation function is used for ameliorate tumor is put, chemotherapy causes side effect, can be used as the adjuvant drug of immunomodulatory and oncotherapy.
But because panaxan's extraction and separating difficulty are bigger, dark by the polysaccharide color that traditional technology is extracted, the main active polysaccharide of its effective constituent (the main galacturonic acid that contains) content is lower, foreign matter content is many, untoward reactions such as irritated and pain often appear in clinical application, therefore, panaxan's extraction process and preparation process are studied, solved above deficiency or defective.
Summary of the invention:
The technical issues that need to address of the present invention just are to overcome the defective of prior art, and a kind of new panaxan's extraction and the method for purifying are provided.
Preparation method of the present invention comprises: the genseng dregs of a decoction sour water after the alcohol extracting is boiled extraction, concentrate behind the extracting liquid filtering, decolouring, alcohol precipitation must precipitate after filtration or after centrifugal, is panaxan's crude product, panaxan's crude product obtains panaxan's extract through after the desalting treatment.
The panaxan's extract that obtains can be made into injection liquid, powder injection or other formulation.
The technical scheme that adopts is:
A kind of panaxan's preparation method of extract is characterized in that comprising following processing step:
Get the genseng meal, add 8-10 and doubly measure 60%～80% alcohol reflux 2-3 time, filter, dregs of a decoction Ex-all ethanol, the dregs of a decoction add 10～15 times of purified water, add hydrochloric acid again, and regulating the pH value is 1～3, decocted 0.5～2 hour, filter, the dregs of a decoction repeat to decoct 1 time, united extraction liquid, filter, concentrating under reduced pressure must extract concentrated solution, and concentrated solution is 1～3 with the salt acid for adjusting pH value, the hydrogen peroxide that adds 4～6 times of hydrochloric acid contents, stir, be incubated 1～3 hour down, be cooled to room temperature at 85～95 ℃, filter, the back concentrated solution must decolour; Decolouring back concentrated solution is regulated pH to 3～5 with NaOH, adds 2～5 times of ethanol, stirs, leave standstill, leaching precipitation, precipitation are with 60～80% washing with alcohol that contain 0.2～2.0%HCl once, the throw out water dissolution repeats alcohol precipitation and acid alcohol washing 1 time, obtains white person gracilis polysaccharide extract.
The white polyoses extract of above-mentioned panaxan's preparation method of extract preparation adds 4～10 times of amounts of injection water and makes dissolving, filters, filtrate 105-130 ℃ was heated 0.1～1.0 hour, filter, the gac of filtrate adding 0.1～0.5% boiled 15 minutes, filtered, add 0.1～1.0 ‰ EDTA-2Na, with the filtering with microporous membrane of 0.1 μ m～0.45 μ m, embedding promptly gets ginseng polysaccharide injection, every milliliter contains the panaxan in galacturonic acid, must not be less than 3.0mg.
Adopt the white polyoses extract of above-mentioned a kind of panaxan's preparation method of extract preparation, with 5～50 parts of described white person gracilis polysaccharide extracts, add 50～95 parts of freeze-dried excipients, make the freeze dried ginseng polysaccharide powder agent, wherein, described freeze-dried excipient is the mixture of the acid of neutral nitrogen base or neutral amino acids and N.F,USP MANNITOL; 50～100 parts of neutral amino acidss, 0～50 part in N.F,USP MANNITOL; Described neutral amino acids is glycine, L-Ala, Serine or proline(Pro).
Adopt the white person gracilis polysaccharide extract of above-mentioned a kind of panaxan's preparation method of extract preparation,, can be made into other various solid preparations by the ordinary method on the pharmaceutics.
Adopt the ginseng polysaccharide injection or the powder injection of above-mentioned a kind of panaxan's preparation method of extract preparation, can be used as intramuscular injection or intravenously administrable; Have the enhancing body immunoloregulation function, be used for ameliorate tumor is put, chemotherapy causes side effect, can be used as the adjuvant drug of immunomodulatory and oncotherapy.
The panaxan extracts research data
1, extraction using alcohol
Adopting orthogonal design, is factor with solvent consumption, alcohol concn, return time, backflow number of times, 3 levels of each factor, and saponin content is an evaluation index among the ginseng residue.Different condition as a result, saponin content is different among the ginseng residue.Conclusion: get the genseng meal, add 10 times of amount 60～80% ethanol, refluxing extraction 2～3 times, each 90min.
2, acid extraction: its principle is to utilize diluted acid that the water-insoluble former panaxan in ginseng crude drug's cell is changed into water-soluble panaxan, adds ethanol or polyvalent metal salt then in extracting solution, the panaxan is precipitated separated out.
1. Suan kind; Carried out simultaneous test with hydrochloric acid, sulfuric acid, acetate, sulfurous acid respectively, the result is best with hydrochloric acid and sulfurous acid effect.But sulfurous acid volatilizes harmful SO
2Gas, therefore contaminate environment adopts hydrochloric acid simultaneously.
2. pH value of solution: in order to obtain the high yield panaxan, respectively with the pH of hydrochloride adjusted solution, be respectively 1.0,1.5,2.0,3.0 and do controlled trial, the result shows that productive rate was the highest between the pH of aqueous extract was controlled at 1.5～2.5.
3. temperature: test shows, extracts temperature below 80 ℃, needs extraction time long, causes the panaxan excessively to take off ester simultaneously.If with water vapor heating more than 100 ℃, though extraction time is short, panaxan's content reduces.Therefore the temperature of extracting preferably is controlled at 90～95 ℃ and is advisable.Acid solution and raw material ratio: all transfer in the liquid phase in order to ensure the soluble human gracilis polysaccharide that extracts, be convenient to filter operation simultaneously, the acid solution consumption should be more greatly.Test shows that acid solution is generally 15: 1 for best with the ratio of raw material.Filter: the filtration of extracting solution is a process comparatively difficult during the panaxan produces.For the ease of filtering, not only to carry out while hot, make flocculating aids with diatomite simultaneously, the panaxan's extracting solution that obtains like this is limpid transparent.
4. solid-liquid ratio: the mass ratio by the HCl of ginseng crude drug and massfraction 0.5% feeds intake at 1: 10, decocts 1.0～1.5h, repeats to extract 1 time, and the panaxan extracts the rate of transform greater than 75%.
3, decolouring
Because acid extraction thing color is darker, contains many non-polysaccharide compounds,, adopt HCl-H in order to remove or destroy this compounds
2O
2Decoloring method.Prove that through simultaneous test concentrated solution is 1～3 with the salt acid for adjusting pH value, add the hydrogen peroxide of 4～6 times of hydrochloric acid contents again, stir insulation (85～95 ℃) down 1～3 hour, be cooled to room temperature, filter, the light yellow clarification concentrated solution in back must decolour.
4, alcohol precipitation and desalination
Because panaxan's molecular weight several ten thousand is to millions of, solubleness is very low in ethanol, adds that alcohol deposition method is convenient to suitability for industrialized production.Because alcohol precipitation postprecipitation thing contains the part metals salt, especially contain calcium salt simultaneously, have a strong impact on the downstream process operation, and the finished product poor stability, precipitation easily separated out.The back concentrated solution is regulated pH to 3～5 with NaOH earlier so will decolour, and adds 2～5 times of ethanol, stirs, leave standstill, leaching precipitation, precipitation are with 60～80% washing with alcohol that contain 0.2～2.0%HCl once, the throw out water dissolution repeats alcohol precipitation and acid alcohol washing 1 time, obtains white polyoses extract.
5, ginseng polysaccharide injection preparation technology
Because panaxan's extract has colloidal property, when heat, destructible colloidal stability produces a large amount of flockss, experimental results show that this precipitates non-polysaccharide compound, belongs to impurity.Investigated the influence of Heating temperature and heat-up time to precipitate for this reason, determine that optimised process is: the extracting waste throw out, add 4～10 times of amounts of injection water and make dissolving, filter, 105～130 ℃ of heating of filtrate 0.1～1.0 hour, filter, the gac of filtrate adding 0.1～0.5% boiled 15 minutes, filter, add 0.1～1.0 ‰ EDTA-2Na, with the filtering with microporous membrane of 0.1 μ m-0.45 μ m, embedding, promptly get ginseng polysaccharide injection, every milliliter contains the panaxan in galacturonic acid, must not be less than 3.0mg.
6, panaxan's preparation of injection
The extracting waste throw out adds 4～8 times of amounts of injection water and makes dissolving, filters, and 105～130 ℃ of heating of filtrate 0.1～1.0 hour are filtered, filtrate is regulated pH to 6.0～7.0 with sodium hydroxide solution, stirs, and adds a small amount of water for injection dilution, stirs evenly, add Serine 120g, stir, filter, filtrate is neutralized to pH6.0～7.0 with hydrochloric acid, add the injection water again to recipe quantity, filter, survey content, packing, 2～5ml/ bottle carries out lyophilize, and outlet seals, gland, lid is rolled in leak detection, labels.
It is simple to extract refining panaxan's method with method of the present invention, operation easily, and it is good to extract purification effect, and the extract color be that white is extremely light yellow, and through assay, the effective constituent galacturonic acid content is higher, and foreign matter content is still less.Prepared ginseng polysaccharide injection more can be given full play to the chemicotherapy effect of its enhancing body immunoloregulation function and antitumor drug, thereby improves patient's quality of life.Be fit to long-term intramuscular injection or intravenous administration.
Embodiment
Embodiment one:
The method for making of ginseng polysaccharide injection:
Get the ginseng crude drug, earlier with 65% alcohol reflux 2 times, dregs of a decoction Ex-all ethanol, the dregs of a decoction add hydrochloric acid again with 12 times of purified water, and regulating the pH value is 2～3, decocted 1.0 hours, and filtered, the dregs of a decoction repeat to decoct 1 time, merge decoction liquor, concentrating under reduced pressure, concentrated solution is 2.0 with the salt acid for adjusting pH value, the hydrogen peroxide that adds 5 times of hydrochloric acid contents again stirs insulation (90～95 ℃) down 1.5 hours, is cooled to room temperature, filter, filtrate is regulated pH to 3～4 with NaOH, adds 3～4 times of ethanol, stirs, leave standstill, the leaching precipitation precipitates with 70% washing with alcohol that contains 1.0%HCl once the throw out water dissolution, repeat alcohol precipitation and acid alcohol washing 1 time, obtain white polyoses extract.Weigh, add 8 times of amounts of injection water and make dissolving, filter, 121 ℃ of heating of filtrate 0.5 hour, filter, the gac of filtrate adding 0.1～0.5% boiled 15 minutes, filtered, add 0.2 ‰ EDTA-2Na, with the filtering with microporous membrane of 0.1 μ m～0.45 μ m, embedding promptly gets ginseng polysaccharide injection, every milliliter contains the panaxan in galacturonic acid, must not be less than 3.0mg.
Embodiment two
The method for making of freeze dried ginseng polysaccharide powder agent:
Get the ginseng crude drug, earlier with 65% alcohol reflux 2 times, dregs of a decoction Ex-all ethanol, the dregs of a decoction add hydrochloric acid again with 12 times of purified water, and regulating the pH value is 2～3, decocted 1.0 hours, and filtered, the dregs of a decoction repeat to decoct 1 time, merge decoction liquor, concentrating under reduced pressure, concentrated solution is 2.0 with the salt acid for adjusting pH value, the hydrogen peroxide that adds 5 times of hydrochloric acid contents again stirs insulation (90～95 ℃) down 1.5 hours, is cooled to room temperature, filter, filtrate is regulated pH to 3～4 with NaOH, adds 3～4 times of ethanol, stirs, leave standstill, the leaching precipitation precipitates with 70% washing with alcohol that contains 1.0%HCl once the throw out water dissolution, repeat alcohol precipitation and acid alcohol washing 1 time, obtain white polyoses extract.Weigh, add 8 times of amounts of injection water and make dissolving, filter, 121 ℃ of heating of filtrate 0.5 hour, filter, filtrate is regulated pH to 6.0～7.0 with sodium hydroxide solution, stirs, and adds a small amount of water for injection dilution, stir evenly, add Serine 120g, stir, filter, filtrate is neutralized to pH6.0～7.0 with hydrochloric acid, adds the injection water again to recipe quantity, filters, and surveys content, packing, the 3.0ml/ bottle carries out lyophilize, outlet, seal, gland is labelled.
Claims (5)
1, a kind of panaxan's preparation method of extract is characterized in that comprising following processing step:
Get the genseng meal, add 8-10 and doubly measure 60%～80% alcohol reflux 2-3 time, filter, dregs of a decoction Ex-all ethanol, the dregs of a decoction add 10～15 times of purified water, add hydrochloric acid again, and regulating the pH value is 1～3, decocted 0.5～2 hour, filter, the dregs of a decoction repeat to decoct 1 time, united extraction liquid, filter, concentrating under reduced pressure must extract concentrated solution, and concentrated solution is 1～3 with the salt acid for adjusting pH value, the hydrogen peroxide that adds 4～6 times of hydrochloric acid contents, stir, be incubated 1～3 hour down, be cooled to room temperature at 85～95 ℃, filter, the back concentrated solution must decolour; Decolouring back concentrated solution is regulated pH to 3～5 with NaOH, adds 2～5 times of ethanol, stirs, leave standstill, leaching precipitation, precipitation are with 60～80% washing with alcohol that contain 0.2～2.0%HCl once, the throw out water dissolution repeats alcohol precipitation and acid alcohol washing 1 time, obtains white person gracilis polysaccharide extract.
2, adopt a kind of according to claim 1 white polyoses extract of panaxan's preparation method of extract preparation, it is characterized in that white person gracilis polysaccharide extract, add 4～10 times of amounts of injection water and make dissolving, filter, filtrate 105-130 ℃ was heated 0.1～1.0 hour, filter, the gac of filtrate adding 0.1～0.5% boiled 15 minutes, filter, add 0.1～1.0 ‰ EDTA-2Na, with the filtering with microporous membrane of 0.1 μ m～0.45 μ m, embedding, promptly get ginseng polysaccharide injection, every milliliter contains the panaxan in galacturonic acid, must not be less than 3.0mg.
3, adopt a kind of according to claim 1 white polyoses extract of panaxan's preparation method of extract preparation, it is characterized in that 5～50 parts of described white person gracilis polysaccharide extracts, add 50～95 parts of freeze-dried excipients, make the freeze dried ginseng polysaccharide powder agent, wherein, described freeze-dried excipient is the mixture of the acid of neutral nitrogen base or neutral amino acids and N.F,USP MANNITOL; 50～100 parts of neutral amino acidss, 0～50 part in N.F,USP MANNITOL; Described neutral amino acids is glycine, L-Ala, Serine or proline(Pro).
4, adopt white person gracilis polysaccharide extract, it is characterized in that, can be made into other various solid preparations by the ordinary method on the pharmaceutics as a kind of panaxan's preparation method of extract preparation as described in the claim 4.
5, adopt as the ginseng polysaccharide injection of a kind of panaxan's preparation method of extract preparation as described in the claim 2,3 or 4 or the application of powder injection, it is characterized in that to be used as intramuscular injection or intravenously administrable; Have the enhancing body immunoloregulation function, be used for ameliorate tumor is put, chemotherapy causes side effect, can be used as the adjuvant drug of immunomodulatory and oncotherapy.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102146143A (en) * | 2010-02-05 | 2011-08-10 | 吉林省宏久生物科技股份有限公司 | Method for preparing pectin and cellulose from extracting residues of ginseng and American ginseng and application thereof |
| WO2013028140A1 (en) | 2011-08-23 | 2013-02-28 | Eraslan Mustafa | Tribulus terrestris, avena sativa and panax ginseng extract combination |
| CN104911233A (en) * | 2014-03-10 | 2015-09-16 | 东北师范大学 | Method for extracting blood glucose lowering ginseng polysaccharides through enzyme method, and applications of method in food and drugs |
-
2008
- 2008-08-06 CN CNA2008100126485A patent/CN101343330A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102146143A (en) * | 2010-02-05 | 2011-08-10 | 吉林省宏久生物科技股份有限公司 | Method for preparing pectin and cellulose from extracting residues of ginseng and American ginseng and application thereof |
| WO2013028140A1 (en) | 2011-08-23 | 2013-02-28 | Eraslan Mustafa | Tribulus terrestris, avena sativa and panax ginseng extract combination |
| CN104911233A (en) * | 2014-03-10 | 2015-09-16 | 东北师范大学 | Method for extracting blood glucose lowering ginseng polysaccharides through enzyme method, and applications of method in food and drugs |
| CN104911233B (en) * | 2014-03-10 | 2018-04-13 | 东北师范大学 | The extracting method of panaxan a kind of and its application in hypoglycemic drug and food is prepared |
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Open date: 20090114 |