CN101337972A - Process for extracting vincaleuucoblastine from vinca - Google Patents
Process for extracting vincaleuucoblastine from vinca Download PDFInfo
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- CN101337972A CN101337972A CNA2008101310315A CN200810131031A CN101337972A CN 101337972 A CN101337972 A CN 101337972A CN A2008101310315 A CNA2008101310315 A CN A2008101310315A CN 200810131031 A CN200810131031 A CN 200810131031A CN 101337972 A CN101337972 A CN 101337972A
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- vinealeucoblastine
- vlb
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Abstract
The invention discloses a method for extracting catharanthine from vincas. Acid extraction solution containing salts is added in fresh vincas to prepare homogenate, which is processed through solid-liquid separation by adopting a decanter centrifuge after ultrasonic treatment; the pH value of extracting solution is adjusted, and organic solvent is used for extracting; then extract liquor is processed through concentration and purification to obtain a finished product of catharanthine. The method has the characteristics that the technology is simple, the production period is short, the extraction efficiency is high, no pollution occurs, etc., and the method can be easily applied to production.
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 Vinorelbine.
The method of extracting vinealeucoblastine(VLB) at present from Vinca has:
1. from fresh catharanthus roseus, extract alkaloidal technology, Patent Office of the People's Republic of China's publication number: CN101007033A; Open day: 2007.8.1; Application number: 200610023692.7.This invention relates to a kind of alkaloidal technology of extracting from fresh catharanthus roseus, by making beating → acid adjustment → centrifugal, squeeze the juice → filters → filtrate accent pH → carbon tetrachloride extraction → and concentratedly take out pine and obtain the alkaloid mixture.
2. the high-efficiency method for producing of a 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), by 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 concentrated solution adjust pH → filtration → cavitation suspendible liquid-liquid extraction → concentrated → purifying.
3. from Vinca, extract the novel process of anticancer active constituent, 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 processing 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.Process for the isolation of alkaloid components from the plantVinca Rosea L. technology of separating bio alkali composition (a kind of from Vinca) United States Patent Office (USPO) 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 processing method of extracting vinca alkaloids by different pH.Raw material obtains alkaloid 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 objective of the invention is to provide that a kind of technical process is simple, extraction yield is high, the method for extracting vinealeucoblastine(VLB) from Vinca of environmentally safe at the deficiencies in the prior art.
In order to achieve the above object, the technical solution used in the present invention is: fresh catharanthus roseus is added to extract in the solution make homogenate, solid-liquid separation is carried out in homogenate after ultrasonication, extracting solution is through adjust pH, organic solvent extraction, and extraction liquid is again through concentrating, obtaining the vinealeucoblastine(VLB) finished product behind the purifying.
Advantage of the present invention:
1. technical process is simple, is easy to promote environmentally safe.
2. the employing ultrasonic extraction has advantage with short production cycle, that extraction yield is high.
3. processing method provided by the invention also can be used for extracting other alkaloid that Vinca contains such as vindoline, Catharanthine, F 81097, vincristine(VCR) etc.
Embodiment
Embodiment is described in further detail the present invention below in conjunction with indefiniteness.
The method of from Vinca, extracting vinealeucoblastine(VLB) provided by the present invention, concrete steps are as follows:
(1), the aquatic foods product that obtain after the Vinca over-ground part cradled, extract solution and add simultaneously and carry out homogenate in the refiner, with 0.5～5% aqueous sulfuric acid the pH value of homogenate is transferred to 1～3.5 then.Described extraction solution is the mixing solutions of aqueous sulfuric acid and inorganic salt solution, and wherein the pH of mixing solutions is 1～3.5, and the volumetric molar concentration of inorganic salt is 0.5M～3.5M.Described inorganic salt are one or two or more kinds mixing wherein of sodium-chlor, Repone K, sodium sulfate or vitriolate of tartar.
(2), be the ultrasonication homogenate of 20KHz～1MHz with the frequency with the ultrasonic extraction machine, to increase the stripping quantity of vinealeucoblastine(VLB), the time is 10～90 minutes.
(3), adopt the centrifugal solid matter of removing of settling centrifuge to obtain extracting solution, separating factor is 1000～6000,3～20 minutes time.
(4), the pH value of extracting solution is transferred to 7.5～12, extract with organic solvent then with strong aqua.Described organic solvent is an ethyl acetate.
(5), extraction liquid is concentrated into the dried vinealeucoblastine(VLB) mixture that obtains under 35～50 ℃ of temperature, negative pressure 0.06～0.1MPa or normal pressure.
(6), the vinealeucoblastine(VLB) mixture is carried out purifying, used elutriant is the chloroform soln that contains 1～10% methyl alcohol with normal phase silicagel column.Carry out wash-out with elutriant, merge the elutriant that contains vinealeucoblastine(VLB) then, under 35～50 ℃ of temperature, negative pressure 0.06～0.1MPa condition, reclaim solvent and obtain the vinealeucoblastine(VLB) crude product.
(7), gained vinealeucoblastine(VLB) crude product is carried out recrystallization and promptly get the vinealeucoblastine(VLB) product; Used recrystallization solvent is 85%～95% methyl alcohol or ethanolic soln.
Embodiment one,
(the pH value is 2.5 aqueous sulfuric acid with the bright Vinca 50kg of water ratio 83% and extracting solution, containing 1M sodium-chlor) 100L mixes and to drop into refiner simultaneously and carry out homogenate, homogenate transfers to pH 2.5 with 2% aqueous sulfuric acid, homogenate is squeezed into the ultrasonic extraction machine through rotor pump, 25KHz ultrasonication 30 minutes, homogenate are centrifugal in rotor pump is squeezed into settling centrifuge again, separating factor 3000,10 minutes time, collect supernatant liquor.Throw out is added new extracting solution repeat aforesaid operations 3 times, merge supernatant liquor, with strong aqua adjust pH to 8～9, place extractor with the ethyl acetate of 1/4 volume, stir extraction 10 minutes, left standstill 10 minutes, is that 30 ℃, negative pressure are that the solvent thickener of 0.1MPa reclaims ethyl acetate with acetic acid ethyl acetate extract through temperature, extraction liquid is concentrated into dried, after crystallization and purification on normal-phase silica gel column chromatography for separation, obtains the vinealeucoblastine(VLB) 1.05g of purity 98.9 again through recrystallization.
Embodiment two,
(the pH value is 1.5 aqueous sulfuric acid with the Vinca 50kg of water ratio 45% and extracting solution, containing 2M sodium sulfate) 100L mixes and to drop into refiner simultaneously and carry out homogenate, homogenate transfers to pH 1.5 with 2% aqueous sulfuric acid, homogenate is squeezed into the ultrasonic extraction machine through rotor pump, 1MHz ultrasonication 30 minutes, homogenate are centrifugal in rotor pump is squeezed into settling centrifuge again, separating factor 3000,5 minutes time, collect supernatant liquor.Throw out is added new extracting solution repeat aforesaid operations 3 times, merge supernatant liquor, transfer pH8～9 with strong aqua, place extractor with the ethyl acetate of 1/4 volume, stir extraction 15 minutes, left standstill 10 minutes, is that 30 ℃, negative pressure are that the solvent thickener of 0.1MPa reclaims ethyl acetate with acetic acid ethyl acetate extract through temperature, extraction liquid is concentrated into dried, after crystallization and purification on normal-phase silica gel column chromatography for separation, obtains the vinealeucoblastine(VLB) 1.33g of purity 98.1 again through recrystallization.
Claims (5)
1, a kind of method of from Vinca, extracting vinealeucoblastine(VLB), it is characterized in that: concrete steps are as follows:
(1), the aquatic foods product that obtain after the Vinca over-ground part cradled, extract solution and add simultaneously and carry out homogenate in the refiner, with 0.5～5% aqueous sulfuric acid the pH value of homogenate is transferred to 1～3.5 then; Described extraction solution is the mixing solutions of aqueous sulfuric acid and inorganic salt solution, and wherein the pH of mixing solutions is 1～3.5, and the volumetric molar concentration of inorganic salt is 0.5M～3.5M;
(2), with the ultrasonic extraction machine be the ultrasonication homogenate of 20KHz～1MHz with the frequency;
(3), adopt the centrifugal solid matter of removing of settling centrifuge to obtain extracting solution, separating factor is 1000～6000,3～20 minutes time;
(4), the pH value of extracting solution is transferred to 7.5～12, extract with organic solvent then with strong aqua;
(5), extraction liquid is concentrated into the dried vinealeucoblastine(VLB) mixture that obtains under 35～50 ℃ of temperature, negative pressure 0.06～0.1MPa or normal pressure;
(6), the vinealeucoblastine(VLB) mixture is carried out purifying, used elutriant is the chloroform soln that contains 1～10% methyl alcohol with normal phase silicagel column; Carry out wash-out with elutriant, merge the elutriant that contains vinealeucoblastine(VLB) then, under 35～50 ℃ of temperature, negative pressure 0.06～0.1MPa condition, reclaim solvent and obtain the vinealeucoblastine(VLB) crude product;
(7), gained vinealeucoblastine(VLB) crude product is carried out recrystallization and promptly get the vinealeucoblastine(VLB) product.
2, the method for extracting vinealeucoblastine(VLB) from Vinca according to claim 1, it is characterized in that: described inorganic salt are one or two or more kinds mixing wherein of sodium-chlor, Repone K, sodium sulfate or vitriolate of tartar.
3, the method for extracting vinealeucoblastine(VLB) from Vinca according to claim 1, it is characterized in that: the time of described ultrasonication homogenate is 10～90 minutes.
4, the method for extracting vinealeucoblastine(VLB) from Vinca according to claim 1, it is characterized in that: described organic solvent is an ethyl acetate.
5, the method for extracting vinealeucoblastine(VLB) from Vinca according to claim 1, it is characterized in that: used recrystallization solvent is 85%～95% methyl alcohol or ethanolic soln.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102372731A (en) * | 2011-11-24 | 2012-03-14 | 广州瑞尔医药科技有限公司 | Preparation method for vinblastine |
| CN102432630A (en) * | 2011-11-18 | 2012-05-02 | 上海安体康生植物化学有限公司 | Method for extracting dehydrated vinblastine and epoxy vinblastine from fresh grass of catharanthus roseus |
| CN104262362A (en) * | 2014-09-01 | 2015-01-07 | 海南希源化工科技有限公司 | Vinblastine extraction and purification method |
| CN104370911A (en) * | 2014-12-13 | 2015-02-25 | 海南希源化工科技有限公司 | Catharanthine tartrate preparation method |
| CN105801605A (en) * | 2014-12-27 | 2016-07-27 | 辽宁药联制药有限公司 | Method for extracting vincristine from catharanthus roseus |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1218950C (en) * | 2004-02-18 | 2005-09-14 | 东北林业大学 | High effect production method of catharanthine |
| CN101007033A (en) * | 2006-01-26 | 2007-08-01 | 杨大耀 | Extraction technology of alkaloids from fresh catharanthus roseus |
-
2008
- 2008-08-12 CN CN2008101310315A patent/CN101337972B/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432630A (en) * | 2011-11-18 | 2012-05-02 | 上海安体康生植物化学有限公司 | Method for extracting dehydrated vinblastine and epoxy vinblastine from fresh grass of catharanthus roseus |
| CN102432630B (en) * | 2011-11-18 | 2014-06-11 | 上海安体康生植物化学有限公司 | Method for extracting dehydrated vinblastine and epoxy vinblastine from fresh grass of catharanthus roseus |
| CN102372731A (en) * | 2011-11-24 | 2012-03-14 | 广州瑞尔医药科技有限公司 | Preparation method for vinblastine |
| CN104262362A (en) * | 2014-09-01 | 2015-01-07 | 海南希源化工科技有限公司 | Vinblastine extraction and purification method |
| CN104370911A (en) * | 2014-12-13 | 2015-02-25 | 海南希源化工科技有限公司 | Catharanthine tartrate preparation method |
| CN105801605A (en) * | 2014-12-27 | 2016-07-27 | 辽宁药联制药有限公司 | Method for extracting vincristine from catharanthus roseus |
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| CN101337972B (en) | 2010-09-15 |
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