CN101693022A - Method for preparing resveratrol sustained-release capsule capable of preventing rheumatoid arthritis - Google Patents
Method for preparing resveratrol sustained-release capsule capable of preventing rheumatoid arthritis Download PDFInfo
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- CN101693022A CN101693022A CN200910197751A CN200910197751A CN101693022A CN 101693022 A CN101693022 A CN 101693022A CN 200910197751 A CN200910197751 A CN 200910197751A CN 200910197751 A CN200910197751 A CN 200910197751A CN 101693022 A CN101693022 A CN 101693022A
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Abstract
The invention relates to a method for preparing resveratrol sustained-release capsule preventing rheumatoid arthritis, which comprises the steps: crushing Polygonum cuspidatum powder to obtain crude powder of 10-30 meshes, adding cellulase liquid, carrying out pretreatment, then using alcohol for reflux extraction, then using macropore absorptive resin for separation, pouring water and alcohol for elution, then adding active carbon for decoloring, and finally using alcohol for repeated crystallization to obtain resveratrol; and respectively preparing quick-release granules and sustained-release granules, mixing the two granules by a mass ratio of 1:1, filling the capsules, thus obtaining the resveratrol sustained-release capsule. The preparation method has simple operation, wide raw material sources and low cost and is environment-friendly; and cellulase is added during the preparation process for pretreatment, therefore, the transferring rate of effective components is greatly improved, and the purity of the extracted resveratrol is ensured, thus being suitable to industrial production.
Description
Technical field
The invention belongs to the preparation field of resveratrol pharmaceutical preparation, particularly a kind of preparation method with resveratrol sustained-release capsule of the rheumatoid arthritis of preventing and treating.
Background technology
Resveratrol (Resveratrol) be plant be subjected to stress the time self synthetic a kind of phytoalexin, extensively exist in the plant, finding in 72 kind of plant of 21 sections, 31 genus at least now has resveratrol to exist.But from the bibliographical information situation, research at present at most, paid close attention to most have only a few Chinese herbal medicine and edible plants such as Rhizoma Polygoni Cuspidati, Fructus Vitis viniferae, Semen arachidis hypogaeae.
At present, extracting natural resveratrol many is raw material with Chinese crude drug Rhizoma Polygoni Cuspidati (root).Because Chinese medicine Rhizoma Polygoni Cuspidati plantation is easily, output height, price are low, convenient sources, and follow-up resource is secure, and research worker has been done a lot of researchs, as: CN1251361A, a kind of technology of from the Chinese medicine Rhizoma Polygoni Cuspidati, extracting resveratrol; 01126769.0, a kind of method that from Rhizoma Polygoni Cuspidati, prepares resveratrol; 02114583.0 one kind is extracted preparing resveratrol from Rhizoma Polygoni Cuspidati; 03147908.1, a kind of method that from Rhizoma Polygoni Cuspidati, prepares resveratrol; 200510027573.4, from the Chinese herbal medicine Rhizoma Polygoni Cuspidati, prepare the method for resveratrol;
200610161949.5, a kind of from the Chinese medicine Rhizoma Polygoni Cuspidati method of separation and purification polydatin and resveratrol;
200810032067.8, the technology of the resveratrol of dna purity more than 98% from Rhizoma Polygoni Cuspidati; 200710030601.7, a kind ofly from fresh Rhizoma Polygoni Cuspidati, extract, the process of purified resveratrol.But all unresolved suitability for industrialized production of above technology and medicinal problem.
Resveratrol has many-sided health care, has the cardiovascular disease of control, anti-cancer, antiviral and immunoregulation effect, and its effect mainly shows as its anti-oxidation characteristics.In industry extensive application prospects such as medicine, food, cosmetics.In recent years, European and American countries has been developed as it health food listing, and tablet, capsule, oral liquor and other types of formulations are arranged.Recently, domestic some resveratrol products that also occurred are as " day lion vigor capsule ", " Zijin capsule ", " the beneficial rubber capsule of the shellfish that receives " etc.; The existing over thousands of kind of the high-end formulation products of resveratrol (comprising medicine and health product) of American-European approved listing, about 200,000,000 people of global user, and, average speed increment with annual 5000 ten thousand people.The sale of estimating following resveratrol preparation will reach 500,000,000～800,000,000 dollars, form very huge industry.
Because it has the adjusting immunologic function, in the treatment immune disease certain curative effect, the little advantage of side effect are arranged, bibliographical information, 200510031435.3, the application of resveratrol in treatment rheumatoid arthritis, non-infectious inflammation.Yet, do not have to solve preparation and the preparation method that is applied to human body, and the oral dosage of human body.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method with resveratrol sustained-release capsule of the rheumatoid arthritis of preventing and treating, this preparation side is simple to operate, raw material sources are extensive, cost is low, environmentally friendly, in preparation process, add the cellulase pretreatment, improved the rate of transform of effective ingredient greatly, guarantee the purity of the resveratrol of extraction, be fit to suitability for industrialized production.
A kind of preparation method with resveratrol sustained-release capsule of the rheumatoid arthritis of preventing and treating of the present invention comprises:
(1) extraction of resveratrol
Pulverize the Rhizoma Polygoni Cuspidati powder and get 10-30 purpose coarse powder, the solution of the cellulase (commercially available) of adding 0.1-1.0% (W/V) was in 20-40 ℃ of pretreatment 30-60 hour, use alcohol reflux then, extracting solution reclaims ethanol, adds water, separate with macroporous adsorbent resin, impouring water and 15%～75% ethanol carry out eluting again, collect eluent, reclaim ethanol, add the activated carbon decolorizing of 0.1-0.5% (W/V), get resveratrol with the ethanol repeated crystallization at last;
(2) preparation of slow releasing capsule
Immediate-release granules: resveratrol 50-100g, lactose 20-50g and starch 20-50g cross 100 orders respectively, mix homogeneously, and the starch slurry that adds 1-10% is made soft material, crosses 40 mesh sieves, and drying is standby;
Slow-releasing granules: resveratrol 50-100g, hydroxypropyl emthylcellulose 30-60g, methylcellulose 10-50g, lactose 10-20g cross 100 orders, mix homogeneously, 5% alcoholic solution moistening of adding polyvinylpyrrolidone (PVP-K30) respectively, make soft material, cross 40 mesh sieves, drying, standby;
Above-mentioned speed, slow two granules are pressed mass ratio mix filled capsules at 1: 1.
The mass volume ratio of described step (1) Chinese medicine powder and 0.1-1.0% (W/V) cellulase solution is 1g: 1.0-2.0ml;
The consumption of the macroporous adsorbent resin in the described step (1) is 0.5-2 a times of Rhizoma Polygoni Cuspidati opaque amount;
Separation in the described step (1) is meant with D type macroporous adsorptive resins, flow velocity 1L/ minute, is eluted to colourless with deionized water;
Eluting in the described step (1) is meant and successively carries out eluting with 15wt% ethanol and 75wt% ethanol.
The invention provides the method for extracting, separating resveratrol from Rhizoma Polygoni Cuspidati, use the cellulase pretreatment, make resveratrol free glycoside hydrolysis, the reuse alcohol extraction, effective ingredient rate of transform height, impurity is few; Because of the macroporous adsorbent resin good separating effect, cost is low in addition, easily produces, the present invention prepares the main D of use, DA series in the method for resveratrol, determine that the macroporous adsorbent resin consumption is the 0.5-2 optimum amount doubly of medical material amount, fully guarantee to adsorb effective ingredient, reduce the waste of resin.
By to resveratrol to the preventive and therapeutic effect of rat assist agent arthritis, to the preventive effect of rat assist agent arthritis Secondary cases pathological changes, the II Collagen Type VI is caused effect research aspect three of the rat rheumatic arthritis effect researchs etc., prove that this medicine has therapeutical effect preferably aspect treatment of arthritis, zoopery shows no matter rat assist agent arthritis is still had therapeutical effect to rat by the inductive rheumatic arthritis of II Collagen Type VI more, this medical instrument has antiinflammatory, analgesic activity simultaneously.These experiments have proved that fully this medical instrument has a plurality of action target spots, multiple therapeutical effect, are very unique medicines.
Beneficial effect
Preparation side of the present invention is simple to operate, and raw material sources are extensive, and cost is low, and is environmentally friendly, adds the cellulase pretreatment in preparation process, improved the rate of transform of effective ingredient greatly, guaranteed the purity of the resveratrol of extraction, is fit to suitability for industrialized production.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
Dry Rhizoma Polygoni Cuspidati 200kg, be ground into coarse powder (10 order), cellulase solution with 0.1% (medicated powder: enzyme liquid=1g: 1.3ml) pretreatment, 25 ℃, 30 hours, the medicated powder of handling, with ethanol 1200L reflux, extract,, extracting solution reclaims ethanol, adds water, with the pillar of D101-I type macroporous adsorbent resin 200kg, flow velocity 1L/ minute, be eluted to deionized water colourless, reuse 15% ethanol 200L eluting, and with 75% ethanol 500L eluting, collect 75% ethanol elution, reclaim ethanol, the concentrated solution activated carbon decolorizing of 0.1-0.5% (W/V), the ethanol repeated crystallization gets resveratrol 2.2kg.
Embodiment 2
Dry Rhizoma Polygoni Cuspidati 200kg, be ground into coarse powder (20 order), cellulase solution with 0.3% (medicated powder: enzyme liquid=1g: 1.5ml) pretreatment, 30 ℃, 48 hours, the medicated powder of handling, with ethanol 1400L reflux, extract,, extracting solution reclaims ethanol, adds water, with the pillar of D101-I type macroporous adsorbent resin 250kg, flow velocity 1L/ minute, be eluted to deionized water colourless, reuse 15% ethanol 200L eluting, and with 75% ethanol 500L eluting, collect 75% ethanol elution, reclaim ethanol, with the activated carbon decolorizing of 0.1-0.5% (W/V), the ethanol repeated crystallization gets resveratrol 2.4kg.
Embodiment 3
Dry Rhizoma Polygoni Cuspidati 200kg, be ground into coarse powder (30 order), cellulase solution with 0.5% (medicated powder: enzyme liquid=1g: 1.8ml) pretreatment, 35 ℃, 60 hours, the medicated powder of handling, with ethanol 1600L reflux, extract,, extracting solution reclaims ethanol, adds water, with the pillar of D101-I type macroporous adsorbent resin 300kg, flow velocity 1L/ minute, be eluted to deionized water colourless, reuse 15% ethanol 200L eluting, and with 75% ethanol 500L eluting, collect 75% ethanol elution, reclaim ethanol, with the activated carbon decolorizing of 0.1-0.5% (W/V), the ethanol repeated crystallization gets resveratrol 2.5kg.
Embodiment 4
The resveratrol sustained-release capsule quality standard
[prescription]: every contains resveratrol 120mg.
Immediate-release granules:
Slow-releasing granules:
[preparation technology]
Immediate-release granules; Principal agent and adjuvant are crossed 100 orders respectively, and mix homogeneously is made soft material with 5% starch slurry, crosses 40 mesh sieves, and drying is standby.
Slow-releasing granules; Principal agent and adjuvant are crossed 100 orders respectively, and mix homogeneously with the moistening of an amount of PVP-K305% alcoholic solution, is made soft material, crosses 40 mesh sieves, and drying is standby.
With speed, slow two granules, five equilibrium mixes, and fills No. 1 capsule, every 0.3g.
[character] capsule, content are that white is to off-white color graininess, mildly bitter flavor.
[discriminating] gets this product content 0.1g, and with ethanol 2ml dissolving, alcoholic solution drops on the filter paper, after the drying, sprays the ferric chloride test solution, shows hyacinthine.
[inspection]
[assay]
Chromatographic condition and system suitability test:
Chromatograph Du: (4.6 * 250mm); Filler is an octadecylsilane chemically bonded silica.
Mobile phase: methanol: water=40: 60;
Flow velocity: 1.0mL/min;
Detect wavelength: 304nm; Sample introduction is: 20 μ L; Column temperature: 25 ℃.
Number of theoretical plate calculates by the resveratrol peak should be not less than 2500.
The preparation of reference substance solution: precision takes by weighing resveratrol reference substance 5mg, adds methanol and makes the solution that every 1ml contains 50 μ g, promptly.
The preparation of need testing solution: get 10 of this product, take out content, precision takes by weighing 30mg, puts the 100ml measuring bottle, adds methanol to scale, shakes up, and gets 1ml, puts the 20ml measuring bottle, adds methanol to scale, promptly.
Algoscopy: accurate respectively reference substance solution and each 20 μ l of need testing solution (filtering) of drawing with micropore (0.45m), inject chromatograph of liquid, measure, promptly.
Every of this product contains resveratrol (C
14H
12O
3) meter, should be in 108-132mg.
[indication] is applicable to adult's rheumatoid arthritis, and the effect of the state of an illness of improvement is arranged.
[usage and consumption] each 1,2 times on the one.Or follow the doctor's advice.
[specification] every 0.3g, 24/box (bottle).
[storage] sealing.
Embodiment 5
Resveratrol (090701) pharmacokinetic parameter (using DAS 2.1.1 to calculate)
Claims (5)
1. preparation method with resveratrol sustained-release capsule of the rheumatoid arthritis of preventing and treating comprises:
(1) extraction of resveratrol
Pulverize the Rhizoma Polygoni Cuspidati powder and get 10-30 purpose coarse powder, the solution of the cellulase of adding 0.1-1.0% (W/V) was in 20-40 ℃ of pretreatment 30-60 hour, use alcohol reflux then, extracting solution reclaims ethanol, adds water, separate with macroporous adsorbent resin, impouring water and 15%～75% ethanol carry out eluting again, collect eluent, reclaim ethanol, add the activated carbon decolorizing of 0.1-0.5% (W/V), get resveratrol with the ethanol repeated crystallization at last;
(2) preparation of slow releasing capsule
Immediate-release granules: resveratrol 50-100g, lactose 20-50g and starch 20-50g cross 100 orders respectively, mix homogeneously, and the starch slurry that adds 1-10% is made soft material, crosses 40 mesh sieves, and drying is standby;
Slow-releasing granules: resveratrol 50-100g, hydroxypropyl emthylcellulose 30-60g, methylcellulose 10-50g, lactose 10-20g cross 100 orders respectively, mix homogeneously, 5% alcoholic solution moistening of adding polyvinylpyrrolidone, make soft material, cross 40 mesh sieves, drying, standby;
Above-mentioned speed, slow two granules are pressed mass ratio mix filled capsules at 1: 1.
2. a kind of preparation method with resveratrol sustained-release capsule of the rheumatoid arthritis of preventing and treating according to claim 1 is characterized in that: the mass volume ratio of the solution of described step (1) Chinese medicine powder and 0.1-1.0% (W/V) cellulase is 1g: 1.0-2.0ml.
3. a kind of preparation method with resveratrol sustained-release capsule of the rheumatoid arthritis of preventing and treating according to claim 1, the consumption that it is characterized in that the macroporous adsorbent resin in the described step (1) are 0.5-2 times of Rhizoma Polygoni Cuspidati opaque amount.
4. a kind of preparation method according to claim 1 with resveratrol sustained-release capsule of the rheumatoid arthritis of preventing and treating, it is characterized in that the separation in the described step (1) is meant with D type macroporous adsorptive resins, flow velocity 1L/ minute, be eluted to colourless with deionized water.
5. a kind of preparation method with resveratrol sustained-release capsule of the rheumatoid arthritis of preventing and treating according to claim 1, it is characterized in that eluting in the described step (1) is meant successively carries out eluting with 15wt% ethanol and 75wt% ethanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101977516A CN101693022B (en) | 2009-10-27 | 2009-10-27 | Method for preparing resveratrol sustained-release capsule capable of preventing rheumatoid arthritis |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101977516A CN101693022B (en) | 2009-10-27 | 2009-10-27 | Method for preparing resveratrol sustained-release capsule capable of preventing rheumatoid arthritis |
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| CN101693022A true CN101693022A (en) | 2010-04-14 |
| CN101693022B CN101693022B (en) | 2011-08-24 |
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| CN2009101977516A Expired - Fee Related CN101693022B (en) | 2009-10-27 | 2009-10-27 | Method for preparing resveratrol sustained-release capsule capable of preventing rheumatoid arthritis |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102920902A (en) * | 2011-11-03 | 2013-02-13 | 青岛康地恩药业股份有限公司 | Avian colibacillosis treatment traditional Chinese medicine and preparation method thereof |
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2009
- 2009-10-27 CN CN2009101977516A patent/CN101693022B/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102920902A (en) * | 2011-11-03 | 2013-02-13 | 青岛康地恩药业股份有限公司 | Avian colibacillosis treatment traditional Chinese medicine and preparation method thereof |
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