CN1029820C - Preparaing technology of extracted substance of Lei Gong gambogl and its beta-ring dextrin envelop matter - Google Patents
Preparaing technology of extracted substance of Lei Gong gambogl and its beta-ring dextrin envelop matter Download PDFInfo
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- CN1029820C CN1029820C CN90105973A CN90105973A CN1029820C CN 1029820 C CN1029820 C CN 1029820C CN 90105973 A CN90105973 A CN 90105973A CN 90105973 A CN90105973 A CN 90105973A CN 1029820 C CN1029820 C CN 1029820C
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- radix tripterygii
- tripterygii wilfordii
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Abstract
The present invention relates to a preparing technology for a tripterygium wilfordii extract and a beta-cyclodextrin inclusion compound thereof. Firstly, the root, the root bark, the stems, the leaves or the other parts of the tripterygium wilfordii are extracted by water, and then, water extraction liquid is extracted by trichloromethane. After the trichloromethane is recovered, the tripterygium wilfordii extract is obtained. Subsequently, the extract is prepared into an ethanol solution (solution A), and the beta-cyclodextrin is prepared into a water solution (solution B). The solution A is added into the hot solution B under a stirring condition. After the solution A and the solution B are treated by thermal insulation, stirring and cooling, the beta-cyclodextrin inclusion compound of the tripterygium wilfordii extract is separated. The beta-cyclodextrin inclusion compound has obvious therapeutic effects on rheumatoid arthritis, chronic nephrosis, lupus erythematosus, psoriasis, etc., and has small toxic side effects.
Description
The present invention relates to the preparation technology of the extract and the Benexate Hydrochloride thereof of Chinese crude drug.Specifically, be the preparation technology of a kind of Radix Tripterygii Wilfordii extract and Benexate Hydrochloride thereof.
The Chinese crude drug Radix Tripterygii Wilfordii is the Celastraceae tripterygium plant, it comprises Radix Tripterygii Wilfordii (Tripterygium wilfordii.Hook.f.), Tripterygium hypoglaucum (T.hypoglaucum(Level) Hutch), black climing (T.regeli Sprague et Takeda) and good fortune Lai Shi Radix Tripterygii Wilfordii (T.forresti Dicls).Radix Tripterygii Wilfordii is used for the treatment of that kind of an immune disease has significant curative effect surplus rheumatoid arthritis, chronic nephropathy, lupus erythematosus, the psoriasis etc. 30.Mainly contain effective constituent and be Diterpenes component based on Radix Tripterygii Wilfordii lactone alcohol.It is at present oral that what be used as medicine is the root of Radix et Rhizoma Tripterygii or peeling, though the aerial parts of tripterygium plant such as stem, leaf, flower, fruit also have obvious curative effects, Radix Tripterygii Wilfordii lactone alcohol content also beguine is much higher, but toxicity is bigger, all give it up at present (seeing " research of Radix Tripterygii Wilfordii and clinical practice " 23-24 page or leaf Li Ruilinshu daf chief editor, China Science Tech Publishing House's JIUYUE in 1989 1 edition).
The extraction process of Radix Tripterygii Wilfordii active ingredient, general at present the employing: water and chloroform extraction, use column chromatography centimetre (seeing " pharmacy circular " 1988 the 23rd volumes the 1st phase page 3) then, or ethanol extraction, reclaim ethanol, technologies such as residue ethyl acetate extraction, recovery ethyl acetate.The operation of these processes is miscellaneous, time-consuming, and yield is wayward, and should not to prepare with water with the extract of gained be the several formulations of solvent.
It is higher to the purpose of this invention is to provide the simple yield of a kind of extraction, the Radix Tripterygii Wilfordii extract that aerial partss such as the root of Radix Tripterygii Wilfordii, root bark and stem, leaf, flowers and fruits can both utilize and the preparation technology of Benexate Hydrochloride thereof.
The present invention is made up of following steps:
With root, root bark, stem, leaf or the other parts extracting in water of tripterygium plant, the aqueous extract organic solvent extraction, the aqueous extract after being extracted returns in the crude drug and extracts, and extracts so repeatedly and extraction, until extracting fully.Organic extract liquid obtains Radix Tripterygii Wilfordii extract after organic solvent is reclaimed in distillation.Then Radix Tripterygii Wilfordii extract is made into 2-15%(weight) ethanol or acetone soln (A liquid).Beta-schardinger dextrin-is made into 2-20%(weight) aqueous solution (B liquid).Under agitation A liquid is joined lentamente in the B liquid of heat, add follow-up continuation of insurance temperature, stir.Cooling is settled out the Benexate Hydrochloride of Radix Tripterygii Wilfordii extract then, filters out clathrate, uses a small amount of organic solvent washing, and decompression is dry down, promptly gets the Benexate Hydrochloride finished product of Radix Tripterygii Wilfordii extract.
Concrete extraction process is: tripterygium wilfordii root, root bark, stem, leaf or other parts are ground into coarse powder, the water temperature that adds 5-10 times of weight is soaked or the percolation extraction, the extracting solution adverse current is by organic solvent extractions such as chloroform or dichloromethane, aqueous extract returns in the medical material and goes, repeat again to extract and extraction, until extracting fully, the chloroform equal solvent is reclaimed in distillation, promptly gets Radix Tripterygii Wilfordii extract.Measure through the many batches of extracts, every Cray Tripterygium wilfordii cured leaf can carry about Radix Tripterygii Wilfordii lactone alcohol 50 micrograms, every Cray Tripterygium wilfordii root bark can carry about Radix Tripterygii Wilfordii lactone alcohol 40 micrograms, show the quality of medical material and decide.
Extract preparation technology can be designed to extract continuously extraction, Fig. 1 be continuous extraction, extract stream and sketch map.The Radix Tripterygii Wilfordii Chinese crude drug is put into extraction pot (1) to be soaked, extracting solution constantly enters extractor (3) by pipeline (2) through filter (12), extractor (3) is composed in series by some column extracting tubes (4), puts into chloroform to scale in each extracting tube (4).Extracting solution enter extractor (3) through the chloroform counter-current extraction after liquid trap (14) enters extracting solution basin (5); Constantly extracting solution is returned the extraction pot (1) from extracting solution basin (5) with pump (6), control valve (9) and pump equate both flows, make extraction effect the best.Meanwhile, chloroform constantly enters extractor (3) through chloroform pipeline (8) from last-extracting tube (4) of extractor (3) from chloroform storage bucket (7), after flowing into chloroform extraction liquid, liquid trap (13) stores bucket (10) by extractor (3) extraction, control valve (11) makes the flow velocity of chloroform reach the optimum efficiency of extraction.
The clathrate process of beta-schardinger dextrin-is: it is 2-15%(weight that Radix Tripterygii Wilfordii extract is made into concentration with alcohol or acetone, as follows), optium concentration is the solution (A liquid) of 5-10%, and it is 2-20% that beta-schardinger dextrin-is made into concentration, and optium concentration is the aqueous solution (B liquid) of 10-15%.Under agitation, A liquid is added to lentamente in 40-80 ℃ the B liquid of 4-6 times of volume, adding follow-up continuation of insurance temperature stirred 2-4 hour, put cold or cold preservation, complete to the cyclodextrin clathrate precipitation, sucking filtration, and with the washing of small amount of acetone or ether, drying under reduced pressure promptly gets the clathrate finished product, and Diterpenes composition such as Radix Tripterygii Wilfordii lactone alcohol of about 90% enters into cyclodextrin and by enclose in the Radix Tripterygii Wilfordii extract.
Advantage of the present invention is that the extraction extraction process is simple; Aqueous extract recycles, and has reduced the consumption of water; With organic solution agent such as chloroform extraction extracting solution, avoided the decocting and concentrating process of extracting solution, the destruction that has prevented the Radix Tripterygii Wilfordii active ingredient well, the also retortable less recovery of consumption of organic solvent such as chloroform; Technology provided by the invention, the Benexate Hydrochloride that promptly uses the extract of aerial partss such as tripterygium leaf, stem to make, toxicity is very little, and is evident in efficacy.We make the cyclodextrin clathrate sheet with Radix Tripterygii Wilfordii extract, and every contains chinol 50 micrograms in the Radix Tripterygii Wilfordii, oral, every day three times, and each two, disease 50 examples such as treatment rheumatoid arthritis, effective percentage is 95%, side effect is minimum.
The present invention be advantageous in that beta-schardinger dextrin-has fabulous hydrophilic, therefore after terpenoid liposoluble constituent such as Radix Tripterygii Wilfordii lactone alcohol is made cyclodextrin clathrate, can be fully soluble in water, being convenient to make injection, oral liquid etc. is the preparation of solvent with water, also be convenient to tabletting, also suitable fully to other dosage form.
Fig. 1 is the sketch map that Radix Tripterygii Wilfordii is extracted extraction process flow continuously.
Below be embodiment.
Embodiment 1
Tripterygium leaf adds 5～6 times of amounts of water, soaked overnight.Leachate is through the chloroform counter-current extraction, and the aqueous extract after the extraction is back in the medical material.So repeatedly circulation is until extracting fully.After chloroform solution reclaims chloroform, get Radix Tripterygii Wilfordii extract.
Embodiment 2
The velamen of Tripterygium wilfordii coarse powder, it is moistening to add water, in the percolator of packing into, adds the suitable quantity of water soaked overnight, begins percolation next day, collects 5 times of amount percolates of medical material, and through the dichloromethane counter-current extraction, extract is back in the percolator again.So repeatedly circulation, until extraction fully.Dichloromethane solution reclaims solvent, promptly gets Radix Tripterygii Wilfordii extract.
Embodiment 3
It is A liquid that Radix Tripterygii Wilfordii extract is made into 2% solution with 95% ethanol, and it is B liquid that the heating of beta-schardinger dextrin-water is made into 5% solution.25 milliliters of A liquid are added in 100 milliliters of B liquid, and 40 ℃ of heated and stirred 2 hours, clathrate was separated out in cold preservation, and sucking filtration with an amount of ether washing, is drained, the dried solvent that volatilizees, drying under reduced pressure, clathrate 4.4 restrains, yield is 81%, the Radix Tripterygii Wilfordii lactone alcohol yield is 86.8%.
Embodiment 4
It is A liquid that Radix Tripterygii Wilfordii extract is made into 10% solution with 95% ethanol, and it is B liquid that the heating of beta-schardinger dextrin-water is made into 10% solution.20 milliliters of A liquid are added in 100 milliliters of B liquid, 80 ℃ of heated and stirred 3 hours, put coldly, placement is spent the night, sucking filtration is with an amount of ether washing, the dried solvent that volatilizees, drying under reduced pressure, pulverize, promptly get clathrate 9.2 grams, yield is 79%, and the yield of Radix Tripterygii Wilfordii lactone alcohol is 90.4%.
Embodiment 5
It is A liquid that Radix Tripterygii Wilfordii extract is made into 15% solution with acetone, and it is B liquid that the heating of beta-schardinger dextrin-water is made into 20% solution, and 15 milliliters of A liquid are added in 100 milliliters of B liquid, 60 ℃ of heated and stirred 4 hours, put coldly, spend the night, separate out clathrate, sucking filtration, with the proper amount of acetone washing, dried solvent volatilizees, drying under reduced pressure, pulverize, get clathrate 19.2 grams, yield is that 84% Radix Tripterygii Wilfordii lactone alcohol yield is 92.5%.
Claims (5)
1, a kind of preparation technology of Benexate Hydrochloride of Radix Tripterygii Wilfordii extract, it is characterized in that root with tripterygium plant, root bark, stem, leaf or other parts extracting in water, the aqueous extract organic solvent extraction, aqueous extract after being extracted returns in the crude drug and extracts, extract so repeatedly and extraction, until extracting fully, organic extract liquid obtains Radix Tripterygii Wilfordii extract after organic solvent is reclaimed in distillation, then Radix Tripterygii Wilfordii extract is made into ethanol or the acetone soln (A liquid) of 2-15% (weight), beta-schardinger dextrin-is made into the aqueous solution (B liquid) of 2-20% (weight), under agitation A liquid is joined lentamente in the B liquid of heat, add follow-up continuation of insurance temperature, stir, cooling is settled out the Benexate Hydrochloride of Radix Tripterygii Wilfordii extract then, filters out clathrate, uses a small amount of organic solvent washing, decompression is dry down, promptly gets the Benexate Hydrochloride finished product of Radix Tripterygii Wilfordii extract.
2, preparation technology according to claim 1 is characterized in that root, root bark or the stem of Radix Tripterygii Wilfordii should be processed into coarse powder, and the consumption of aqueous extract is 5～10 times of weight of dried medical material, and extracting method can be used warm macerating, or percolation
3, according to claim 1 and 2 described preparation technologies, the organic solvent that it is characterized in that extracting usefulness can be chloroform or dichloromethane, can extract with counter-current extraction.
4, according to claim 1 and 2 described preparation technologies, it is characterized in that under agitation A liquid being joined lentamente in 40-80 ℃ the B liquid, add follow-up continuation of insurance temperature, stirred 2-4 hour, A liquid optium concentration is 5-10%, the optium concentration of B liquid is 10-15%, and the optimum volume ratio of A, B liquid is 1: 4-1: 6.
5, preparation technology according to claim 3, it is characterized in that under agitation A liquid being joined lentamente in 40-80 ℃ the B liquid, add follow-up continuation of insurance temperature and stirred 2-4 hour, the optium concentration of A liquid is 5-10%, the optium concentration of B liquid is 10-15%, and the optimum volume ratio of A, B liquid is 1: 4-1: 6.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN90105973A CN1029820C (en) | 1990-11-15 | 1990-11-15 | Preparaing technology of extracted substance of Lei Gong gambogl and its beta-ring dextrin envelop matter |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN90105973A CN1029820C (en) | 1990-11-15 | 1990-11-15 | Preparaing technology of extracted substance of Lei Gong gambogl and its beta-ring dextrin envelop matter |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1051859A CN1051859A (en) | 1991-06-05 |
| CN1029820C true CN1029820C (en) | 1995-09-27 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN90105973A Expired - Fee Related CN1029820C (en) | 1990-11-15 | 1990-11-15 | Preparaing technology of extracted substance of Lei Gong gambogl and its beta-ring dextrin envelop matter |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1055629C (en) * | 1996-05-07 | 2000-08-23 | 侯树英 | Making up method for medicinal liquid of ice guide therapeutic method on channels and acupuncture point |
| CN1079101C (en) * | 1999-02-03 | 2002-02-13 | 中国科学院广州化学研究所 | Prepn. of cassia oil and beta-cyclodextrin indusion compound |
| US8003139B2 (en) | 2002-04-09 | 2011-08-23 | Sichuan Institute Of Chinese Materia Medica | Pharmaceutical composition for treating rheumatism, and method of making same |
| CN115025026B (en) * | 2022-06-07 | 2023-10-03 | 清远市望莎生物科技有限公司 | Natural plant extract composition with relieving, repairing and anti-allergic effects |
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- 1990-11-15 CN CN90105973A patent/CN1029820C/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| CN1051859A (en) | 1991-06-05 |
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