CN1431215A - Method for preparing glucoside in resveratrol of medicine to nourish liver and lowering fat - Google Patents
Method for preparing glucoside in resveratrol of medicine to nourish liver and lowering fat Download PDFInfo
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- CN1431215A CN1431215A CN 03117246 CN03117246A CN1431215A CN 1431215 A CN1431215 A CN 1431215A CN 03117246 CN03117246 CN 03117246 CN 03117246 A CN03117246 A CN 03117246A CN 1431215 A CN1431215 A CN 1431215A
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Abstract
A liver-protecting hypolipemic compound, resveratrol glucoside, is prepared from giant knotweed rhizome through crushing, decocting, adding alcohol, stirring, deposition removing alcohol, extracting with acetate solvent, water washing, removing organic solvent, dissolving in alcohol, cooling while crystallizing, filtering, and washing with ice water. It can be used in conjunction with pharmacological recepatable assistant and/or additive to prepare relative medicine.
Description
Technical field
What the present invention relates to is a kind of extract for preparing natural medicinal plant, and with the preparation method of this extract as the liver-protecting and blood fat-reducing medicine of active drug composition.
Background technology
Polidatin, chemical name are 3,4, and 5-resveratrol-3-list-glycoside is a kind of composition with medical active that is contained in the natural medicinal plant giant knotweed.In to its chemical ingredients and Pharmacological action study document, Zhang Xiyun is in " Tianjin pharmacy " 1999, having reported polidatin contained in the giant knotweed in 11 (8) can be by reducing blood-fat, expansion arteriole, increase the effect of aspects such as heartbeat output and pulse pressure difference, inhibition flow of calcium ions, resisting pathogenic microbes, bring into play many-sided physiology and pharmacologically active effect to human body." herbal medicine communication " 1974,9 (2) " about the research of Rhizoma Polygoni Cuspidati treatment chronic tracheitis effective constituent " and " contemporary Chinese application pharmacy " 1999, in 16 (5) documents such as " the anti-herpes virus hominis's researchs of giant knotweed ethyl acetate extraction part ", also the medicinal use of Rhizoma Polygoni Cuspidati extract is reported to some extent.Can also be recognized by these documents, be the method that raw material extracts wherein contained polidatin with the giant knotweed at present, can have alcohol extracting-water precipitating shallow lake method and water extracting alcohol precipitation method several.Wherein, the cost of alcohol extracting-water precipitating shallow lake method is higher, complex process, and the production cycle is longer; And in the water extracting alcohol precipitation method that above-mentioned document is reported, after aqueous extract done the precipitation removal of impurities and handle with ethanol, all need handle again with benzene, and then extract with ethyl acetate.The toxicity of benzene is well-known.With handling with benzene in the medicine leaching process, not only increased cost, also significantly increased difficulty of post-processing, also increased the unsafe factor of final medicine simultaneously.
Summary of the invention
At above-mentioned situation, it is raw material with the giant knotweed that the present invention will propose a kind of, and preparation does not particularly use benzene as the method for extracting solvent when extracting polidatin as the method for effective medicinal ingredients polidatin of liver-protecting and blood fat-reducing medicine.Another purpose of the present invention, be to be the active drug composition by the polidatin that obtains with described method, further prepare commonly used as oral drug preparations such as solid types such as capsule, tablet, granule, liquid-type or slow release types, and the method for the liver-protecting and blood fat-reducing medicine of several formulations form such as injection.
The present invention prepares the method for liver-protecting and blood fat-reducing medicine polidatin, obtains polidatin with organic solvent extraction again after needing equally to adopt decocting extracting solution to the dry rhizome of natural medicinal plant giant knotweed with ethanol sedimentation.Wherein, the decocting of the giant knotweed dry rhizome meal after pulverizing is got extracting solution, and to add ethanol to the whole content of the ethanol in the solution be 60%-65% and stir precipitation, it is that the acetic ester solvent of 97%-99% fully extracts that residuum content behind the ethanol (after recyclable again utilize) is removed in decompression, and after washing the acetic ester extracting solution with water, the organic solvent of removing in the acetic ester extracting solution (utilizing again after recyclable) obtains medicinal extract, use also cooling, the crystallization of dissolve with ethanol of 55%-65% again, filter back frozen water washing precipitation, obtain polidatin, pulverize the back and use for preparation.
In above-mentioned preparation method, extract that the said residuum that decompression is removed behind the ethanol extracts used acetic ester solvent in the polidatin process, can be in vinyl acetic monomer, propyl acetate or the N-BUTYL ACETATE commonly used any.Test-results shows, to the residue medicinal extract thing after removing the organic solvent in the acetic ester extracting solution again with the dissolve with ethanol of 55%-65% and when carrying out crystallisation by cooling, the effect that this alcoholic acid usage quantity is the medicinal extract volume 4-5 times the time is generally comparatively satisfied.
Resulting polidatin has better color and luster in the aforesaid method in order to make, can be behind the said medicinal extract that obtains in by the acetic ester extracting solution with the dissolve with ethanol of 55-65%, adopt earlier and the sorbing material that in pharmacy, allows to use---as sorbing materials commonly used such as the pharmaceutical gac 30-40 minute after-filtration that reflux jointly, will carry out crystalline deposit after the filtrate cooling again.
The polidatin that obtains with aforesaid method is effective medicinal ingredients, after it is pulverized, by present usual manner be added in the medicine acceptable corresponding auxiliary and/added ingredients after, can further be prepared into operational pharmaceutical preparation.These pharmaceutical preparations can include multi-form oral preparations, also can be injection formulationss.For example, be added in the oral preparations behind the corresponding auxiliary interpolation material of acceptable by present usual manner, can be prepared into the capsule, tablet, granule of corresponding solid type or its any in preparation of corresponding slow release formulation separately, or the preparation of drink form.Be added in the corresponding auxiliary interpolation material of acceptable in the injection formulations as further preparation requirement, and after mode is handled in accordance with regulations, can be prepared into corresponding injection type, for example contain jumbo injection by injection.
Wherein, test-results shows, when preparing above-mentioned solid type oral preparations, if on the basis of above-mentioned polidatin as the active drug composition, the 3-8 giant knotweed raw material fine powder doubly that further adds granularity again and be 180 ± 7.6 microns, consumption and be polidatin weight mixes and uses, and jointly as the active drug composition, but also can make the effect of its performance thinner, and reduce cost, thereby has even more ideal effect.In oral dosage form, adopt with the fine powder of an amount of giant knotweed raw material superiority to be, both can make its effect of bringing into play thinner, also utilized its crude drug cheaply to be easy to get aptly and reach the purpose that reduces cost as auxiliary added ingredients mode.
With preparation capsule preparations medicine is example, will extract as stated above and obtain polidatin, further by the routine requirement of preparation pharmaceutical capsules with operate, and comprises thinners such as starch, lactose, Microcrystalline Cellulose, hydroxypropylcellulose; Lubricant such as Magnesium Stearate, talcum powder; And the auxiliary interpolation material that uses during preparation capsules such as retarding agent such as polyvinylpyrrolidone, and granularity be 180 ± 7.6 microns, consumption be polidatin weight 3-3.5 giant knotweed raw material fine powder mixed together doubly evenly after, granulate, after the drying, by needed dose filling capsule.
In above-mentioned pharmaceutical preparation, for the content specification of preparation, general recommendations is adopted: the solid type medicine can be the 4-60 milligram for each drug particles unit contains polidatin; Oral liquid is the 1-30 mg/ml; Injection is the 1-30 mg/ml.
Owing to got rid of use among the above-mentioned preparation method of the present invention to noxious solvent benzene, guaranteed simultaneously the high-content of resulting polidatin again, problems have been simplified because of using benzene that subsequent disposal is brought, shortened the production cycle, also fundamentally eliminate the hidden danger that causes the medicine insecurity, helped making quality product to be guaranteed reliably.
Below form by embodiment again foregoing of the present invention is described in further detail, but this should be interpreted as that the scope of the above-mentioned theme of the present invention only is confined to following embodiment.All technology that realizes based on foregoing of the present invention all belong to scope of the present invention.
Embodiment
Example 1
500 gram giant knotweed exsiccant rhizomes were ground into the meal of 1-2 number sieve of Chinese Pharmacopoeia regulation, and the decocting that adds 8 times of amounts boils tapping after 1 hour, filters with 80 mesh sieves; The dregs of a decoction add 6 times of water gagings again and decocted 1 hour, and the same manner filters.Merging filtrate, heating are concentrated into relative density 1.20-1.25 (heat is surveyed).After cold slightly, add content and be 95% ethanol, the whole content of the ethanol of regulator solution is 60%～65%, stirs to place and spends the night.Behind supernatant liquid filtering, decompression recycling ethanol also is condensed into the nearly medicinal extract of doing.With separating funnel content is 1000 milliliters * 4 pairs medicinal extract thing joltings extractions of vinyl acetic monomer of 97%-99%, separates.Behind the united extraction liquid, water 1000 milliliters * 4 gradation joltings washing.The vinyl acetic monomer solution decompression is reclaimed solvent to nearly dry extract shape.Adding content is 60% ethanol, and heating stirs, and adds a little gac backflow decolouring in 30-40 minute, cold slightly after-filtration.Separate out crystal after the filtrate cooling, filter, frozen water repetitive scrubbing crystal after drying gets polidatin, and products obtained therefrom is detected.
Detected result: fusing point is 146-147 ℃;
Ultimate analysis: C55.64 (calculated value 56.34%), H6.28% (calculated value 6.15%);
Ultra-violet absorption spectrum: λ
Hexanol265nm (lg ε) 216 (4.32), shoulder 230 (4.39),
303(4.55)，318(4.52)；
Infrared absorption spectrum (KBr sheet, cm
-1): 3400 (hydroxyls), 1600,1525,1470 (phenyl ring),
1270,1185 (phenyl ring δ C-H), 1160 (phenolic hydroxyl group C=O),
1100,1040 (hydroxyl on the sugar, C=O), 970 (HC=CH-),
850 (1,4-two replacements and 1,3,5-trisubstituted benzene ring).
Example 2
Get the above-mentioned polidatin that obtains 15 grams, starch 90 grams, lactose 80 grams, Microcrystalline Cellulose 35 grams, hydroxypropylcellulose 20 grams mix, cross 100 mesh sieves three times, add 10% polyvinylpyrrolidone (PVP) ethanolic soln and make softwood for 100 milliliters, 24 mesh sieves are granulated, dry below 60 ℃, the whole grain of 24 mesh sieves, adding accounts for the Magnesium Stearate of gross weight 1%, 1% talcum powder respectively, after mixing, fill with No. 2 capsules, every loading amount 0.25 gram is made 1000.
Example 3
Ingredient proportion is: polidatin 15 grams, and starch 30 grams,
Low-substituted hydroxypropyl cellulose 15 grams, Microcrystalline Cellulose 20 grams,
The 10%PVP ethanolic soln is an amount of, micropowder silica gel 2 grams,
Magnesium Stearate 2 grams are made 1000 altogether.
Behind the above-mentioned polidatin that obtains by example 1 method and starch, low-substituted hydroxypropyl cellulose, the common mixing of Microcrystalline Cellulose, adding the 10%PVP ethanolic soln stirs, make into softwood, granulate with 20 order nylon mesh, 60 ℃ of dryings, whole grain is behind adding micropowder silica gel, the Magnesium Stearate mixing, compressing tablet, the bag film-coat.
Example 4
After 500 gram giant knotweed exsiccant rhizomes being ground into the meal of 1-2 number sieve of Chinese Pharmacopoeia regulation, by the same quadrat method of above-mentioned example 1 with aqueous extract with Ethanol Treatment after, use ethyl acetate extraction again, granulate to add an amount of dextrin and sweeting agent by the nearly dry extract shape thing that obtains behind the ethyl acetate extraction liquid decompression and solvent recovery, dry, whole grain can become the particle drug form.
Example 5
Get polidatin 15 grams that obtained with quadrat method by example 1, add an amount of back of dextrin and sweeting agent and granulate, drying also can obtain corresponding particle drug form.
Example 6
1.5 gram tween-80s are dissolved in the proper amount of water for injection, add polidatin 15 grams and the dissolving fully that obtain with quadrat method by example 1 again, be configured to 1000 milliliters with water for injection, regulate pH6.6-7.0, injection preparation requires to use respectively 3G sintered glass funnel and millipore filtration (0.45 μ m) to filter routinely, in the canned 2ml ampoule of going into to contain rare gas element, and sealing by fusing, the sterilization leak detection promptly obtains injection medicine.
Claims (10)
1. the method for preparing liver-protecting and blood fat-reducing medicine polidatin, the decocting extracting solution of the dry rhizome of natural medicinal plant giant knotweed is obtained polidatin with organic solvent extraction after with ethanol sedimentation again, it is characterized in that decocting with the giant knotweed dry rhizome meal after pulverizing gets extracting solution and adds ethanol to the whole content of the ethanol in the solution and be 60%-65% and stir, precipitation and filtration, it is that the acetic ester solvent of 97%-99% fully extracts that residuum content behind the ethanol is removed in decompression, and after washing the acetic ester extracting solution with water, the organic solvent of removing in the acetic ester extracting solution obtains medicinal extract, use the dissolve with ethanol of 55%-65% again, cooling, crystallization, filter back frozen water washing precipitation, obtain polidatin, pulverize the back and use for preparation.
2. preparation method as claimed in claim 1 is characterized in that saidly residuum behind the ethanol being removed in decompression to extract used acetic ester solvent being in vinyl acetic monomer, propyl acetate, the N-BUTYL ACETATE any.
3. preparation method as claimed in claim 1, when it is characterized in that remaining medicinal extract thing behind the said organic solvent of removing in the acetic ester extracting solution with the dissolve with ethanol of 55%-65% and crystallization, the alcoholic acid usage quantity be the medicinal extract volume 4-5 doubly.
4. preparation method as claimed in claim 1, it is characterized in that with the dissolve with ethanol of 55%-65% said by behind the medicinal extract that obtains in the acetic ester extracting solution, after the sorbing material that adds permission use in the pharmacy refluxes jointly and also filtered in 30-40 minute, again with filtrate cooling and crystallization.
5. preparation method as claimed in claim 4 is characterized in that the sorbing material that allows in the said pharmacy to use is gac.
6. being the method that effective medicinal ingredients prepares the liver-protecting and blood fat-reducing medicine by the polidatin that obtains as one of claim 1 to 5 method, it is characterized in that after the resulting polidatin pulverizing, be added in the medicine acceptable corresponding auxiliary and/added ingredients after, be prepared into operational pharmaceutical dosage form.
7. process for preparing medicine as claimed in claim 6, it is characterized in that after the resulting polidatin pulverizing, doubly measure with its weight 3-8, granularity is that 180 ± 7.6 microns giant knotweed raw material fine powder mixes, common active drug composition during as preparation solid dosage oral pharmaceutical.
8. process for preparing medicine as claimed in claim 7 is characterized in that prepared solid type medicine is the 4-60 milligram for each drug particles unit contains polidatin.
9. preparation method as claimed in claim 6 is characterized in that with resulting polidatin be the active drug composition, is prepared into the oral liquid that the trans-resveratrol salidroside content is the 1-30 mg/ml.
10. preparation method as claimed in claim 6 is characterized in that being prepared into the injection type that the trans-resveratrol salidroside content is the 1-30 mg/ml with resulting polidatin.
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| CNB031172466A CN1182149C (en) | 2003-01-27 | 2003-01-27 | Method for preparing glucoside in resveratrol of medicine to nourish liver and lowering fat |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007068171A1 (en) * | 2005-12-13 | 2007-06-21 | Shenzhen Neptunus Pharmaceutical Holdings Co., Ltd. | CRYSTALLINE FORM I OF 3,4',5-TRIHYDROXY-STIBENE-3-β-D-GLUCOSIDE |
| WO2007131444A1 (en) * | 2006-05-15 | 2007-11-22 | Shenzhen Neptunus Pharmaceutical Holdings Co., Ltd. | New crystallographic form of the compound 3,4',5-trihydroxyl-stilbene-3-beta-d-glucoside |
| CN101613385B (en) * | 2006-05-15 | 2011-09-21 | 深圳海王药业有限公司 | Crystal form of 3,4',5-trihydroxy stilbene-3-beta-D-glucoside |
| CN102453059A (en) * | 2010-10-17 | 2012-05-16 | 陕西理工学院 | Method for extracting polydatin from giant knotweed with inorganic solvent |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1977852B (en) * | 2005-12-07 | 2010-04-21 | 周亚伟 | Medicinal composition containing stilbene total glycoside and its use for pharmaceutical treating hepatitis B |
-
2003
- 2003-01-27 CN CNB031172466A patent/CN1182149C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007068171A1 (en) * | 2005-12-13 | 2007-06-21 | Shenzhen Neptunus Pharmaceutical Holdings Co., Ltd. | CRYSTALLINE FORM I OF 3,4',5-TRIHYDROXY-STIBENE-3-β-D-GLUCOSIDE |
| CN100432090C (en) * | 2005-12-13 | 2008-11-12 | 深圳海王药业有限公司 | I crystal form 3, 4', 5-trihydroxy-3-beta-D-heteroside |
| US8575115B2 (en) | 2005-12-13 | 2013-11-05 | Shenzhen Neptunus Pharmaceutical Holdings Co., Ltd. | Crystalline form I of 3,4′5-trihydroxy-stilbene-3-β-D glucoside |
| WO2007131444A1 (en) * | 2006-05-15 | 2007-11-22 | Shenzhen Neptunus Pharmaceutical Holdings Co., Ltd. | New crystallographic form of the compound 3,4',5-trihydroxyl-stilbene-3-beta-d-glucoside |
| CN100516080C (en) * | 2006-05-15 | 2009-07-22 | 深圳海王药业有限公司 | 3,4', 5-trihydroxystilbene-3-beta-D-glucoside crystal form |
| CN101613385B (en) * | 2006-05-15 | 2011-09-21 | 深圳海王药业有限公司 | Crystal form of 3,4',5-trihydroxy stilbene-3-beta-D-glucoside |
| CN102453059A (en) * | 2010-10-17 | 2012-05-16 | 陕西理工学院 | Method for extracting polydatin from giant knotweed with inorganic solvent |
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| CN1182149C (en) | 2004-12-29 |
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