CN1345716A - Process for extracting and separating anthraquinone compound from Chinese herbal medicinal material - Google Patents
Process for extracting and separating anthraquinone compound from Chinese herbal medicinal material Download PDFInfo
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- CN1345716A CN1345716A CN 00125406 CN00125406A CN1345716A CN 1345716 A CN1345716 A CN 1345716A CN 00125406 CN00125406 CN 00125406 CN 00125406 A CN00125406 A CN 00125406A CN 1345716 A CN1345716 A CN 1345716A
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Abstract
In present invention an adsoption process with macroporous adsorption resin is used instead of organic solvent extraction process to purify and refine anthraquinones compound from crude extract of traditional Chinese herbal medicine. Its total anthraquinone content is greater than or equal to 50%. It avoids the use of toxic and harmful solvent, and is simple in operation process, low in cost, easy to control in product quality, and is applicable to large-scale production.
Description
The present invention relates to extraction of effective components in the plant amedica, be specifically related to the method for extraction, separating anthraquinone compound from plant amedica.
Anthraquinone (anthraquinone) is the general name that has as the compound of lower skeleton.
Anthraquinone analog compound has comprised the product and the dipolymer of its different reducing degrees, as anthrol (anthranol), Oxanthrone (oxanthranol), anthrone (anthrone), DIANTHRAQUINONE (dianthraquinone), dianthrone (dianthrone) etc., also has the glucoside of these compounds in addition.In natural product, anthraquinone often is present in the meta-bolites of polygonaceae, pulse family, Rubiaceae and lower plant lichens and mushroom of higher plant.Modern pharmacological research proves that anthraquinone analog compound has very strong biological activity and pharmacological action.Mainly contain 1. anastalsis: anthraquinone analog compound can promote thrombocyte to generate, and obviously increases Fibrinogen, and the clotting time is shortened, and reduces capillary permeability, improves vascular fragility, makes active the increasing of contraction of blood vessel, therefore can promote blood coagulation.2. anti-microbial effect: anthraquinone analog compound all has in various degree restraining effect to various bacteria, and wherein the most responsive with staphylococcus, suis, dysentery bacterium, diphtheria corynebacterium, Bacillus subtilus and Corynebacterium diphtheriae etc. are also responsive.Antifungal mechanism mainly is to suppress the oxidation and the dehydrogenation of thalline sugar and metabolic intermediate, and can arrestin and nucleic acid synthetic, therefore can avoid the toxic side effects and the resistance of some antibiotic clinically.3. discharge function: the protection of combined anthraquinone glucoside reason glycosyl, most ofly directly arrive large intestine without absorbing, it is first and sugared to be resolved into glucoside by bacterial enzyme in intestines.Glucoside unit stimulates big intestinal mucosa, and suppresses sodium ion and absorb from enteric cavity, makes that moisture increases in the large intestine, and hyperperistalsis and causing is rushed down.4. diuretic properties: anthraquinone analog compound can make the urine amount increase, and promotes ureteral wriggling, and sodium potassium also obviously increases in the urine, and produces the diuretic antihypertensive effect.Its effect is by reducing the amino acid whose heavy absorption of enteron aisle, urea is synthetic in the inhibition hepatic and renal tissue, improve free indispensable amino acid concentration in the blood, utilize blood urea nitrogen compound body albumen in the body and suppress the decomposition of myoprotein, and increase that the drainage of urea and creatinine finishes.In addition, along with the research of basic theory deepens continuously, for the clinical application of anthraquinone analog compound provides theoretical foundation.The Chinese medicine preparation application clinically that contains anthraquinone analog compound has related to many treatment of diseases, as treating severe crisis and miscellaneous diseases such as coronary heart disease, mucosal ulcer, lymphoid tuberculosis, burn and scald, chronic gastritis, acute cholecystitis, injury of the bone section disease, acute cerebrovascular disease.
The anthraquinone derivative that exists in the plant amedica mostly is hydroxyanthraquinone and their glucoside.Most anthraquinone glycoside is that the hydroxyl and the sugared condensation of anthraquinone forms, and it is that sugared carbon atom with anthraquinone directly is formed by connecting that minority is also arranged.Usually the combined anthraquinone molecular weight is less than 500, and water-soluble and organic solvent, the dissociated anthraquinone molecular weight is about about 300, is soluble in organic solvent as ether, chloroform, benzene, ethanol etc., also dissolve in the alkaline aqueous solution as ammoniacal liquor, sodium hydroxide solution etc., and water insoluble.At present, extracting the product that contains anthraquinone analog compound from natural product mainly is the crude extract of herbal medicine, and the total anthraquinones content of crude extract is not more than 20%.The refining normal organic solvents such as ether, benzene, chloroform that use of anthraquinone analog compound in the herbal medicine are though the total anthraquinones content of gained Chinese medical concrete can reach more than 50%.But these organic solvents are inflammable and explosive poisonous and harmful reagent, do not control well and can cause very major injury to human body as solvent residual amount in the medicinal extract, and this method is dangerous big, environment are also had to pollute be not suitable for scale operation.
The objective of the invention is to provide a kind of easy and simple to handle, safe, pollution-free, cost is low, the anthraquinone analog compound selectivity height that extracts from plant amedica, the separating and extracting method that active constituent content is high.
The present invention extracts from plant amedica, the method for separating anthraquinone compound is realized by the following step:
The crude drug that will contain anthraquinone analog compound extracts with usual method and obtains the effective constituent crude extract, get crude extract and add water, transfer pH to 6.5-10 with alkaline solution, join in the adsorption column that macroporous adsorbent resin is housed, crude extract amount (g) and amount of resin (ml) are than being 1: 10-100; Through macroporous adsorptive resins absorption, with water and elutriant wash-out, collect elutriant, concentrate, be drying to obtain the medicinal extract that contains anthraquinone analog compound, total anthraquinones content 〉=50%.
Crude extract of the present invention be meant the crude drug that contains anthraquinone analog compound with ordinary method through water or organic solvent extraction, remove the dregs of a decoction, extracting solution suitably concentrates or directly is concentrated into drying effective component extracts.The also available method for refining commonly used of crude extract carries out pre-treatment.Crude extract anthraquinone total content is 5-30%.
Alkaline solution of the present invention is meant alkaline aqueous solutions such as sodium hydroxide, potassium hydroxide, ammoniacal liquor.
Macroporous adsorbent resin of the present invention is macroporous adsorbent resins such as styrene type, 2-methacrylate type, and granularity is that 10～100 orders, specific surface area are 100～800cm
2/ g, aperture 10～400 .
Elutriant of the present invention is meant the mixed solution of alkaline aqueous solutions such as methyl alcohol, ethanol, acetone, ethyl acetate and their mixed solution and sodium hydroxide, potassium hydroxide, ammoniacal liquor and alkaline aqueous solution and above-mentioned organic solvent.
Upper prop mode of the present invention also earlier with the crude extract organic solvent dissolution, is admixed macroporous adsorbent resin dry powder, then upper prop behind the pressure reducing and steaming organic solvent.Wherein said organic solvent is meant methyl alcohol, ethanol, acetoneand ethyl acetate etc.
The macrolattice sorbent material is a new technology that grows up the seventies.Be used for fields such as wastewater treatment, medicine industry, analytical chemistry, clinical identification and treatment abroad the earliest.China begins to use macroporous adsorbent resin at the end of the seventies and extracts, separates the herbal medicine chemical ingredients.
Macroporous adsorbent resin is generally white form of spherical particles, and physico-chemical property is stable, is insoluble to acid, alkali and organic solvent.Organism is selected better the influence that not existed by inorganic salts and strong ion low molecular compound.Macroporous adsorbent resin is the parting material that adsorptivity and screening property principle combine, and is different with the ion exchange resin separation principle of using in the past.The adsorptivity that itself has is because the result of Van der Waals force or generation hydrogen bond.Sieve property principle is because itself cellular structure determines.Just because of these characteristics, make organic compound especially the purification of water-soluble cpds simplified greatly.From in shape micro-, macroporous adsorbent resin includes many netted opening structures that the microcosmic bead is formed that have.What made by the very little monomer polymerization of moment of dipole when these spheroids is not nonpolar adsorption resin with the polymeric adsorbent of any functional group, for example, and the polymeric adsorbent of vinylbenzene-divinylbenzene system.The hydrophobicity of this class polymeric adsorbent hole surface is stronger, can be by the organism in the interaction adsorbent solution of the hydrophobic part in the small molecules.And the Semi-polarity polymeric adsorbent means the polymeric adsorbent that contains ester group, for example, and crosslinked analog copolymers such as acrylate or methacrylic ester and methacrylate glycol ester, its surface hydrophobicity part and hydrophilic parts coexistence.Polar Adsorbent Resin is meant that amide-containing, itrile group, phenolic hydroxyl group etc. are nitrogenous, the polymeric adsorbent of oxygen, sulphur polar functionalities base.In addition, sometimes the ion exchange resin of ligand groups such as nitrogenous, oxygen, sulphur is called strong Polar Adsorbent Resin.Because adsorptivity and sieve property principle, organic compound separates through certain solvent elution on macroporous adsorbent resin according to the difference of adsorptive power and the size of molecular weight.The present invention is exactly characteristics of having utilized nonpolar and resinene in the macroporous adsorbent resin, and the dissociated anthraquinone in the plant amedica separated and purifying with combined anthraquinone.
The present invention substitutes organic solvent extractionprocess with the absorption with macroporous adsorbent resin method, purification, refined anthracene quinones from the Chinese medicine crude extract, avoid using the poisonous and harmful solvent, operating procedure is simple, cost is low, quality product is easy to control, and is applicable to scale operation.Make that Chinese medicine preparation effective constituent is clear and definite, active constituent content is brought up to higher level, for Chinese medicine preparation move towards the world, moves towards modernization convenience is provided.
Embodiment one: extract anthraquinone analog compound from rheum officinale
(resin structure is styrene type, granularity 20-80 order, specific surface 400cm to get the macroporous adsorbent resin of having handled well
2, aperture 100 ) 120ml, wet method dress post.Other gets rheum officinale crude extract 5g, adds water 100ml, regulates pH to 7-8 with 4% potassium hydroxide, go up sample after the stirring and dissolving, flow velocity 8-15 drips/minute, treat that sample all adds, wash with water almost colourless or faint yellowly no longer change earlier to effluent liquid, change 95% ethanol eluate wash-out, collect alcohol eluen, concentrate, be drying to obtain, total anthraquinones content 〉=58%, yield 〉=3.5%.Embodiment two: extract anthraquinone analog compound from giant knotweed
(resin structure is styrene type, granularity 20-80 order, specific surface 400cm to get the macroporous adsorbent resin of having handled well
2, aperture 100 ) 200ml, wet method dress post.Other gets giant knotweed crude extract 5g, adds water 100ml, regulates pH to 7-8 with 4% sodium hydroxide, go up sample after the stirring and dissolving, flow velocity 8-15 drips/minute, treat that sample all adds, wash with water almost colourless or faint yellowly no longer change earlier to effluent liquid, change eluent ethyl acetate liquid wash-out, collect elutriant, concentrate, be drying to obtain, total anthraquinones content 〉=52%, yield 〉=3.5%.Embodiment three: extract anthraquinone analog compound from Tuber Fleeceflower Root
(resin structure is styrene type, granularity 20-80 order, specific surface 400cm to get the macroporous adsorbent resin of having handled well
2, aperture 100 ) 400ml, wet method dress post.Other gets Tuber Fleeceflower Root crude extract 5g, adds water 100ml, regulates pH to 7-8 with 4% sodium hydroxide, go up sample after the stirring and dissolving, flow velocity 8-15 drips/minute, treat that sample all adds, wash with water almost colourless or faint yellowly no longer change earlier to effluent liquid, change 80% ethanol eluate wash-out, collect alcohol eluen, concentrate, be drying to obtain, total anthraquinones content 〉=55%, yield 〉=3.5%.
Claims (4)
1, a kind ofly from plant amedica, extract, the method for separating anthraquinone compound, this method is that the crude drug that will contain anthraquinone analog compound extracts acquisition effective constituent crude extract with usual method, it is characterized in that getting this crude extract and add water, transfer pH to 6.5-10 with alkaline solution, join in the adsorption column that macroporous adsorbent resin is housed, crude extract amount (g) and amount of resin (ml) are than being 1: 10-100; Through macroporous adsorptive resins absorption, with water and elutriant wash-out, collect elutriant, concentrate, be drying to obtain the medicinal extract that contains anthraquinone analog compound, total anthraquinones content 〉=50%.
2, a kind ofly as claimed in claim 1ly from plant amedica, extract, the method for separating anthraquinone compound, it is characterized in that wherein said macroporous adsorbent resin is macroporous adsorbent resins such as styrene type, 2-methacrylate type, granularity is that 10～100 orders, specific surface area are 100～800cm
2/ g, aperture 10～400 .
3, a kind ofly as claimed in claim 1ly from plant amedica, extract, the method for separating anthraquinone compound, it is characterized in that wherein said elutriant is meant the mixed solution of alkaline aqueous solution such as methyl alcohol, ethanol, acetone, ethyl acetate and their mixed solution and sodium hydroxide, potassium hydroxide, ammoniacal liquor and alkaline aqueous solution and above-mentioned organic solvent.
4, a kind ofly as claimed in claim 1ly from plant amedica, extract, the method for separating anthraquinone compound, it is characterized in that wherein said alkaline solution is meant alkaline aqueous solutions such as sodium hydroxide, potassium hydroxide, ammoniacal liquor.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 00125406 CN1113844C (en) | 2000-09-26 | 2000-09-26 | Process for extracting and separating anthraquinone compound from Chinese herbal medicinal material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 00125406 CN1113844C (en) | 2000-09-26 | 2000-09-26 | Process for extracting and separating anthraquinone compound from Chinese herbal medicinal material |
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| CN1345716A true CN1345716A (en) | 2002-04-24 |
| CN1113844C CN1113844C (en) | 2003-07-09 |
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| CN 00125406 Expired - Fee Related CN1113844C (en) | 2000-09-26 | 2000-09-26 | Process for extracting and separating anthraquinone compound from Chinese herbal medicinal material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102190691A (en) * | 2010-03-17 | 2011-09-21 | 上海医药工业研究院 | Method for preparing high-purity 4'-epi-daunorubicin |
| CN102430002A (en) * | 2011-11-23 | 2012-05-02 | 合肥七星医药科技有限公司 | Patience dock root total anthraquinone medicament for preventing and treating various hemorrhagic diseases and preparations as well as preparation method thereof |
| CN103127251A (en) * | 2012-03-14 | 2013-06-05 | 成都中医药大学 | Overground part extract of rheum officinale, extraction and purification method and use thereof |
| CN105287478A (en) * | 2015-11-09 | 2016-02-03 | 魏芳 | Medicine composition for treating gastritis |
-
2000
- 2000-09-26 CN CN 00125406 patent/CN1113844C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102190691A (en) * | 2010-03-17 | 2011-09-21 | 上海医药工业研究院 | Method for preparing high-purity 4'-epi-daunorubicin |
| CN102190691B (en) * | 2010-03-17 | 2014-08-27 | 上海医药工业研究院 | Method for preparing high-purity 4'-epi-daunorubicin |
| CN102430002A (en) * | 2011-11-23 | 2012-05-02 | 合肥七星医药科技有限公司 | Patience dock root total anthraquinone medicament for preventing and treating various hemorrhagic diseases and preparations as well as preparation method thereof |
| CN103127251A (en) * | 2012-03-14 | 2013-06-05 | 成都中医药大学 | Overground part extract of rheum officinale, extraction and purification method and use thereof |
| CN103127251B (en) * | 2012-03-14 | 2014-10-29 | 成都中医药大学 | Overground part extract of rheum officinale, extraction and purification method and use thereof |
| CN105287478A (en) * | 2015-11-09 | 2016-02-03 | 魏芳 | Medicine composition for treating gastritis |
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| CN1113844C (en) | 2003-07-09 |
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Granted publication date: 20030709 Termination date: 20130926 |