CN102516264A - Method for separating vinblastine by using ion exchange resin - Google Patents
Method for separating vinblastine by using ion exchange resin Download PDFInfo
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- CN102516264A CN102516264A CN2011104032065A CN201110403206A CN102516264A CN 102516264 A CN102516264 A CN 102516264A CN 2011104032065 A CN2011104032065 A CN 2011104032065A CN 201110403206 A CN201110403206 A CN 201110403206A CN 102516264 A CN102516264 A CN 102516264A
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- vinealeucoblastine
- vlb
- vinblastine
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Abstract
The invention discloses a method for separating a Chinese medicine, i.e., vinblastine, and particularly discloses a method for separating vinblastine from a Chinese medicinal vinblastine extracting solution. According to the technical scheme of the invention, the method comprises the following steps of: preparing a vinblastine extracting solution; adjusting the pH value to 2-4; filtering; adding a filtrate onto a cation exchange resin column; eluting and removing impurities by using water; soaking the resin column into a 5-20 percent saline solution; eluting with a 5-20 percent saline solution containing acid or ethanol; checking whether alkaloid exists; collecting an eluent; adding alkali for neutralizing; desalting; and concentrating and drying to obtain Chinese medicinal vinblastine. According to the method, high-purity vinblastine can be efficiently separated from the Chinese medicinal vinblastine extracting solution, the defects of low extraction rate, large using amount of an organic solvent, super high acid and alkali concentrations, complex process and the like existing in the prior art are overcome, and production application is easy.
Description
Technical field
The present invention relates to natural medicine field, particularly a kind of method that adopts ultrasonic wave extraction from Vinca, to extract vinealeucoblastine(VLB).
Background technology
Vinealeucoblastine(VLB) mainly extracts from periwinkle and obtains, and is a kind of anti-cancer alkaloid that the apocynaceae plant Vinca is contained, and is the antitumor drug of present clinical use, also can be used as the chemical intermediate of synthetic another kind of anti-cancer alkaloid VNB.
The method of from Vinca, extracting vinealeucoblastine(VLB) at present has: alkaloidal technology, Patent Office of the People's Republic of China's publication number: CN101007033A are extracted in (1) from fresh catharanthus roseus; Open day: 2007.8.1; Application number: 200610023692.7, this invention relates to a kind of alkaloidal technology of from fresh catharanthus roseus, extracting, and takes out pine through making beating → acid adjustment → centrifugal, the accent pH → carbon tetrachloride extraction of squeezing the juice → filters → filtrate → concentrated and obtains the vegeto-alkali mixture; (2) a kind of high-efficiency method for producing of vinealeucoblastine(VLB), Patent Office of the People's Republic of China's publication number: CN1534038A; Open day: 2004.10.6; Application number: 200410013558.X.This invention relates to a kind of high-efficiency method for producing of vinealeucoblastine(VLB), through Vinca is concentrated through extracting solvent → homogenate liquid-solid extraction → cavitation suspension extraction → filtrations → extracting solution with alcohol or acid alcohol → obtain the vinealeucoblastine(VLB) finished product behind liquid concentrator adjust pH → filtration → cavitation suspendible liquid-liquid extraction → concentrated → purifying; (3) novel process of extraction anticancer active constituent from Vinca, Patent Office of the People's Republic of China's publication number: CN1365978A; Open day: 2002.08.28; Application number: 011319879.9.This invention relates to the process method of extracting vinealeucoblastine(VLB), vincristine(VCR) and ursolic acid in a kind of Vinca herb dry powder, and the winestone acid solution counter-current extraction → acid-soluble material that adopts Vinca siccative abrasive dust → benzene diacolation → 3～10% is through column chromatography for separation → vinealeucoblastine(VLB) and vincristine(VCR); (4) the Process for the isolation of alkaloid components from the plantVinca Rosea L. technology of separating bio alkali composition (a kind of from Vinca) USPO's publication number: 4172077; Open day: 1979.10.23; Application number: [HU] RI 638.This invention relates to a kind of with after the pulverizing of Vinca hay, extracts the process method of extracting vinca alkaloids through different pH.Raw material obtains vegeto-alkali through pulverizing → methyl alcohol, 2% aqueous sulfuric acid and toluene diacolation → concentrated percolate → pH gradient extraction → purifying; Wherein method (2) (3) (4) have that complex process be difficult for to be promoted, extraction time shortcomings such as length, production cost height; There is noxious solvents such as using benzene, toluene, tetracol phenixin in method (1) (3) (4), easily environment is polluted.
Summary of the invention
The method that the purpose of this invention is to provide a kind of safe, low-cost, high efficiency extraction separation Chinese medicine vinealeucoblastine(VLB).
This goal of the invention realizes through following technology: get the extracting solution that contains the Chinese medicine Vinca, adjustment pH value 2 to 4 filters; Getting filtrating and being added on the cation exchange resin column,, soaking resin column with 5%～20% salts solution more earlier with the water elution removal of impurities; Afterwards to contain acid or alcoholic acid salts solution wash-out; Collect elutriant,, promptly get required vinealeucoblastine(VLB) through desalting treatment.
Based on above-mentioned technological process, the contriver has carried out further research again, and the parameter of each step of refinement filters out preferred embodiment, and particular content is following:
The concentration of salt solution of used immersion resin is preferably 10%～15%, and wash-out concentration is preferably 5%～8%.
Used salt can be CaCl
2, KCl, NaCl, NH
4Among the Cl any is preferably NaCl and NH
4Cl.
The time of used salt solution soaking resin is 1～5 hour.
Wash-out contains 0.2～0.5% hydrochloric acid with salts solution or contains 0.2～0.5% sulfuric acid or 10%～30% ethanol.
Used resin can be Hydrogen and salt type, is preferably salt type such as sodium type or ammonium type.
Elution speed is preferably per hour 4～6 times of column volumes.
This technological process compared with prior art, not only technical process is simple, and adopts salts solution (containing diluted acid or rare alcohol) as elutriant; To the basic non-corrosiveness of equipment; The equipment of industrial product is required to have reduced, and cost reduces greatly, more is prone to realize enlarging the purpose of producing.
Embodiment
Below in conjunction with specific embodiment the present invention is done further explain.
Embodiment one
Get Vinca 100g, add the sour water diacolation of pH=4, merge the percolate thin up to 1000ml; Centrifugal, regulate pH=2, centrifugal; Supernatant is with 5 times of column volumes/hour through Zeo-karb (001 * 7, sodium type, blade diameter length ratio 1: 6); Washing to effluent does not have color, and 0.2% hydrochloric acid soln with 10% sodium-chlor soaked resin 5 hours again.Use 0.3% hydrochloric acid soln wash-out of 5% sodium-chlor again; Elution speed be 4 times of column volumes/hour, soaked behind 2 times of column volumes of wash-out 5 hours, be eluted to vegeto-alkali inspection negative (effluent drips 10% silicotungstic acid does not have deposition) again; Collect elutriant; Be neutralized to neutrality with sodium hydroxide, desalination, the filtrating concentrate drying gets vinealeucoblastine(VLB).
Embodiment two
Get Vinca 50g, boiling 2 times, each 10 times of amounts decocted 2 hours; Merge decoction liquor, centrifugal, regulate pH=3; Centrifugal, supernatant with 4 times of column volumes/hour through Zeo-karb (001 * 2.5, the ammonium type; Blade diameter length ratio 1: 8), wash to effluent and do not have color, 0.5% hydrochloric acid soln with 5% ammonium chloride soaked resin 2 hours again.Use 0.2% hydrochloric acid soln wash-out of 5% ammonium chloride again, elution speed be 2 times of column volumes/hour, to vegeto-alkali inspection negative (effluent drips 10% silicotungstic acid does not have deposition); Collect elutriant; Be neutralized to neutrality with sodium hydroxide, desalination, the filtrating concentrate drying gets vinealeucoblastine(VLB).
Embodiment three
Get Vinca 50kg, add 70% ethanol ultrasonic extraction twice, add 5 times of amounts at every turn, ultrasonic 0.5 hour; United extraction liquid, centrifugal, reclaim ethanol, add water to 500ml; Regulate pH=2, centrifugal, supernatant with 2 times of column volumes/hour through last Zeo-karb (001 * 10, the sodium type; Blade diameter length ratio 1: 8), wash to effluent and do not have color, 0.5% hydrochloric acid soln with 20% sodium-chlor soaked resin 1 hour again.Use 0.2% hydrochloric acid soln wash-out of 10% sodium-chlor again, elution speed be 5 times of column volumes/hour, to vegeto-alkali inspection negative (effluent drips 10% silicotungstic acid does not have deposition); Collect elutriant; Be neutralized to neutrality with sodium hydroxide, desalination, the filtrating concentrate drying gets vinealeucoblastine(VLB).
Claims (7)
1. a method of from the Vinca extracting solution, separating vinealeucoblastine(VLB) is characterized in that this method is: get the Vinca extracting solution, regulate pH value 2 to 4; Filter, cross cation exchange resin column, earlier with the washing removal of impurities; Soak resin column with 5%～20% salts solution again, to contain acid or alcoholic acid 5%～20% salts solution wash-out, collect elutriant again; Through desalting treatment, concentrate drying gets vinealeucoblastine(VLB).
2. the method for separation vinealeucoblastine(VLB) according to claim 1 is characterized in that the concentration of salt solution of used immersion resin is preferably 10%～15%, and wash-out concentration is preferably 5%～8%.
3. the method for separation vinealeucoblastine(VLB) according to claim 1 is characterized in that used salt can be CaCl
2, KCl, NaCl, NH
4Among the Cl any is preferably NaCl and NH
4Cl.
4. the method for separation vinealeucoblastine(VLB) according to claim 1, the time that it is characterized in that used salt solution soaking resin is 1-5 hour.
5. the method for separation vinealeucoblastine(VLB) according to claim 1 is characterized in that wash-out contains 0.2～0.5% hydrochloric acid with salts solution or contains 0.2～0.5% sulfuric acid or 10%～30% ethanol.
6. the method for separation vinealeucoblastine(VLB) according to claim 1 is characterized in that used resin can be Hydrogen and salt type, is preferably salt type such as sodium type or ammonium type.
7. the method for separation vinealeucoblastine(VLB) according to claim 1 is characterized in that elution speed is preferably per hour 4～6 times of column volumes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104032065A CN102516264A (en) | 2011-11-25 | 2011-11-25 | Method for separating vinblastine by using ion exchange resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104032065A CN102516264A (en) | 2011-11-25 | 2011-11-25 | Method for separating vinblastine by using ion exchange resin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102516264A true CN102516264A (en) | 2012-06-27 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011104032065A Pending CN102516264A (en) | 2011-11-25 | 2011-11-25 | Method for separating vinblastine by using ion exchange resin |
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|---|---|
| CN (1) | CN102516264A (en) |
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2011
- 2011-11-25 CN CN2011104032065A patent/CN102516264A/en active Pending
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Application publication date: 20120627 |