CN1045784A - Speiss in the camptothecine production process is handled - Google Patents
Speiss in the camptothecine production process is handled Download PDFInfo
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- CN1045784A CN1045784A CN 89101590 CN89101590A CN1045784A CN 1045784 A CN1045784 A CN 1045784A CN 89101590 CN89101590 CN 89101590 CN 89101590 A CN89101590 A CN 89101590A CN 1045784 A CN1045784 A CN 1045784A
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- camptothecine
- speiss
- crude product
- production process
- handled
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Abstract
The invention provides a kind of novel process of handling the speiss that is produced in the camptothecine production process.This technology is that speiss is boiled with saturated limewater earlier, repetitive scrubbing, and wherein water-soluble composition washes as far as possible, improves the camptothecine yield.Useless speiss is handled with liquid caustic again, at first reclaims the camptothecine crude product in the alkali lye, separates obtaining a large amount of Betulinic acids then.The camptothecine crude product that reclaims also must separate through silica gel column chromatography just can reach criterion of acceptability.
Description
The present invention relates to a kind of treatment process, promptly with Fructus Camptothecae Acuminatae (seed) be the processing of the speiss that produced in the process of raw material production antitumor drug camptothecine and the method for recycling.
Root or bark with camplotheca acuminata are the raw material production camptothecine, can not produce speiss; And adopt Fructus Camptothecae Acuminatae (seed) is raw material, a large amount of speiss then occur.Existing production technology is with hot water repetitive scrubbing speiss, so that wherein water soluble component comes out as far as possible.Though also once considered to use the NaOH alkali liquid washing, making the camptothecin molecule structure is sodium salt by the lactone form open loop, increases solubleness, so that improve the rate of recovery of camptothecine.But under alkaline condition, a large amount of foreign material also are dissolved in the aqueous solution, bring bigger difficulty for later operation (filter, concentrate, acidifying, extraction, refining etc.).And in the past when the filtering speiss of superheated water repetitive scrubbing is used as waste residue and is abandoned,, can only shovel in the boiler in batches and burn owing to still contain composition contaminate environment such as camptothecine.
The objective of the invention is to recycle, improve the yield of camptothecine, and make triterpene compound-betulinic acid by adopting technologies such as alkali cleaning, filtration, acidifying, extraction, separation that speiss is handled.
The present invention is achieved in that
With speiss saturated limewater (milk of lime or slaked lime powder and water are formulated) boiling washing 2～4 times that produce in the production camptothecine process, pH value is 8～12, both kept alkalescence, increase the solubleness of camptothecine, do not influence filtration again, later process operations is not had influence, the yield of camptothecine is brought up to more than 0.02% by about 0.01%.
Through the filtering useless speiss of boiling washing repeatedly, use the caustic alkali (NaOH etc.) of 0.01～2% concentration to boil filtration again, after the filtrate neutralization (pH value 5～7), the filtering precipitation, acidifying then (pH value 2～4), use organic solvent extractions such as chloroform, tetracol phenixin, ethyl acetate again, also can obtain partly camptothecine crude product.
The camptothecine crude product that reclaims from useless speiss often contains a large amount of impurity, and (chloroform: fine purification treatment process methyl alcohol 1: 1) is difficult to reach qualified requirement to adopt general mixed solvent.The present invention mixes silica gel with the camptothecine crude product, carries out column chromatography, separates with chloroform solution (1～4%) wash-out that contains methyl alcohol, makes qualified camptothecine crystallization.
Boil the residue filter residue of handling through caustic alkali, be washed with water to neutrality, drying, further refining with organic solvents such as methyl alcohol, ether, chloroforms, can obtain triterpene compound-betulinic acid.
It is that the speiss that raw material carries out in the production of camptothecine industrialness is handled that the present invention is applicable to Fructus Camptothecae Acuminatae (seed), and simple to operate, used liming source easily, and is cheap, nontoxic, improved camptothecine yield (reaching as high as 0.024%) significantly.Contained betulinic acid is an output maximum in the plant origin of finding so far in the useless speiss, continue to handle with liquid caustic, molten decon promptly gets pure product through the organic solvent recrystallization, and can develop becomes a kind of medicine with different physiological roles.
Claims (1)
1, a kind of treatment process to the speiss that produced in the camptothecine production process is characterized in that:
With the speiss boiling washing, keeping pH value is 8～12 with saturated limewater (it is formulated that milk of lime or slaked lime powder add water) for a, elder generation, filters repeatable operation 2～4 times.
B, useless speiss boil, filter with the caustic alkali of 0.01～2% concentration again.
C, alkaline filtrate neutralizing treatment filter out impurities, and organic solvent extractions such as chloroform, tetracol phenixin or ethyl acetate are used in acidifying again (PH2～4) then, and recyclable a part of camptothecine crude product separates qualifiedly the camptothecine crystallization through silica gel column chromatography.
D, boil the residue of handling (filter residue) through caustic alkali, be washed with water to neutrality, drying is used the refining betulinic acid that obtains of organic solvent (methyl alcohol, ether, chloroform etc.) again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89101590 CN1045784A (en) | 1989-03-18 | 1989-03-18 | Speiss in the camptothecine production process is handled |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89101590 CN1045784A (en) | 1989-03-18 | 1989-03-18 | Speiss in the camptothecine production process is handled |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1045784A true CN1045784A (en) | 1990-10-03 |
Family
ID=4854352
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 89101590 Pending CN1045784A (en) | 1989-03-18 | 1989-03-18 | Speiss in the camptothecine production process is handled |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1045784A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101220036B (en) * | 2007-11-09 | 2011-06-15 | 仲恺农业技术学院 | Extraction of active ingredient such as betulinic acid from common camptotheca fruit with clean method |
| CN101347468B (en) * | 2007-07-20 | 2012-01-04 | 天津天士力制药股份有限公司 | Effective component of common camptotheca fruit and preparation as well as use thereof |
| CN102675328A (en) * | 2011-03-17 | 2012-09-19 | 温州大学 | Method for extracting betulinic acid and camptothecin from camptotheca acuminate fruits |
-
1989
- 1989-03-18 CN CN 89101590 patent/CN1045784A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101347468B (en) * | 2007-07-20 | 2012-01-04 | 天津天士力制药股份有限公司 | Effective component of common camptotheca fruit and preparation as well as use thereof |
| CN101220036B (en) * | 2007-11-09 | 2011-06-15 | 仲恺农业技术学院 | Extraction of active ingredient such as betulinic acid from common camptotheca fruit with clean method |
| CN102675328A (en) * | 2011-03-17 | 2012-09-19 | 温州大学 | Method for extracting betulinic acid and camptothecin from camptotheca acuminate fruits |
| CN102675328B (en) * | 2011-03-17 | 2014-11-26 | 温州大学 | Method for extracting betulinic acid and camptothecin from camptotheca acuminate fruits |
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| C53 | Correction of patent for invention or patent application | ||
| CB02 | Change of applicant information |
Address after: Pond river, Nanning, Guangxi Applicant after: Nanning Futuijunren sanatorium welfare factory Address before: South Bridge, Hechi, Guangxi Applicant before: Guangxi Hechi District Technology Development Center Pilot Plant |
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| COR | Change of bibliographic data |
Free format text: CORRECT: APPLICANT; FROM: GUANGXI HECHI DISTRICT TECHNOLOGY DEVELOPMENT CENTER PILOT PLANT TO: NANNING AREA VETERANS NURSING HOME WELFARE FACTORY |
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| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |