CN101643478A - Process for preparing vinblastine - Google Patents
Process for preparing vinblastine Download PDFInfo
- Publication number
- CN101643478A CN101643478A CN200910027239A CN200910027239A CN101643478A CN 101643478 A CN101643478 A CN 101643478A CN 200910027239 A CN200910027239 A CN 200910027239A CN 200910027239 A CN200910027239 A CN 200910027239A CN 101643478 A CN101643478 A CN 101643478A
- Authority
- CN
- China
- Prior art keywords
- vinealeucoblastine
- vlb
- preparation
- acetic acid
- aqueous solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a process for preparing vinblastine, which has simple and convenient operation and less pollution and equipment investment. The process comprises the following steps: soakingthe whole catharanthus roseus by 8-12 times of acetic acid aqueous solution with concentration of 5-20 percent for 2 hours; assisting to extract by a microwave with the extracting power of 600W and the extracting time of 2-8 minutes; filtering and adjusting the pH value of filter liquor to 8 by ammonia water; adsorbing by a macroporous absorption resin column; eluting and removing impurities by 20-60 percent of alcohol with the pH value being equal to 5; eluting by 95 percent of alcohol; concentrating eluent, adding acetone crystals, washing and drying to obtain the vinblastine. The process for preparing the vinblastine is easy to realize industrialization amplification.
Description
Technical field
The present invention relates to a kind of preparation method of vinealeucoblastine(VLB), especially a kind of method of from Vinca, extracting vinealeucoblastine(VLB).
Background technology
Vinealeucoblastine(VLB) (vinblastine) is a kind of dimeric indole Alkaloid with tangible anti-tumor activity that extracts from the apocynaceae plant Vinca.It has significant curative effect to Hodgkin and lung cancer in non-cellule type, malignant lymphoma etc.Year was still one of main tumour medication so far surplus its vitriol had been widely used in clinical 30.Find from Vinca for middle and advanced stage Beer and Johnson etc. and extract vinealeucoblastine(VLB) from nineteen fifty, from Vinca herb 1Kg, isolated 100 surplus kind of indole alkaloid, the content of vinealeucoblastine(VLB) is about 4/100000ths.Mainly be to extract vinealeucoblastine(VLB) from natural phant at present, though utilize chemosynthesis and semisynthetic method can obtain vinealeucoblastine(VLB) and derivative thereof, also the someone studies the approach acquisition by tissue culture, and is all undesirable, is not suitable for producing.So detecting also from natural phant, the technology of separation and Extraction vinealeucoblastine(VLB) just seems important.
In the prior art, extract vinealeucoblastine(VLB) and mainly adopt solvent method and supercritical extraction, the former adopts organic solvent in a large number, and environment is polluted; Latter's equipment has high input, and is unfavorable for industrialization.
Summary of the invention
Technical problem to be solved by this invention provides a kind of easy and simple to handle, equipment and drops into little, as to pollute little vinealeucoblastine(VLB) preparation method.
For solving the problems of the technologies described above, the present invention adopts following technical proposal:
Get the Vinca herb, doubly measuring concentration with 8-12 is that the acetic acid aqueous solution of 5-20% soaked 2 hours, and microwave-assisted extracts, extract power 600W, extraction time 2-8 minute, filter, filtrate is regulated pH to 8 with ammoniacal liquor, the absorption of employing macroporous adsorptive resins, with the 20-60% ethanol elution removal of impurities of pH=5, use 95% ethanol elution again, concentrate eluant, add the acetone crystallization, wash, be drying to obtain.
Extract and be preferably 10% with acetic acid aqueous solution concentration, consumption is preferably 10 times of amounts.
Microwave-assisted extraction time is preferably 4 minutes.
The model of macroporous adsorptive resins is one or more among H-1020, X-5, AB-8, H-103, D-101, DA-201, DS-401, the DM-301.
The macroporous resin wash-out is preferably 50% except that using mixedly alcohol concn.
Adopt technique scheme to prepare vinealeucoblastine(VLB), easy and simple to handle, pollute less, equipment drops into for a short time, is beneficial to big production operation.
Below in conjunction with embodiment the present invention is further elaborated, but the scope of protection of present invention is not limited to following embodiment.
Embodiment
Embodiment 1
Getting Vinca herb 1Kg, is that 5% acetic acid aqueous solution soaked 2 hours with 8 times of amount concentration, and microwave-assisted extracts, extract power 600W, 2 minutes extraction times, filter, filtrate is regulated pH to 8 with ammoniacal liquor, adopts the absorption of H-1020 type macroporous adsorptive resins, with the 20% ethanol elution removal of impurities of pH=5, use 95% ethanol elution again, concentrate eluant adds the acetone crystallization, washs, is drying to obtain vinealeucoblastine(VLB) 0.36g, adopt HPLC to detect, its purity is 97.6%.
Embodiment 2
Getting Vinca herb 1Kg, is that 20% acetic acid aqueous solution soaked 2 hours with 12 times of amount concentration, and microwave-assisted extracts, extract power 600W, 8 minutes extraction times, filter, filtrate is regulated pH to 8 with ammoniacal liquor, adopts the absorption of X-5 type macroporous adsorptive resins, with the 60% ethanol elution removal of impurities of pH=5, use 95% ethanol elution again, concentrate eluant adds the acetone crystallization, washs, is drying to obtain vinealeucoblastine(VLB) 0.48g, adopt HPLC to detect, its purity is 96.7%.
Embodiment 3
Getting Vinca herb 1Kg, is that 10% acetic acid aqueous solution soaked 2 hours with 10 times of amount concentration, and microwave-assisted extracts, extract power 600W, 4 minutes extraction times, filter, filtrate is regulated pH to 8 with ammoniacal liquor, adopts the absorption of AB-8 type macroporous adsorptive resins, with the 50% ethanol elution removal of impurities of pH=5, use 95% ethanol elution again, concentrate eluant adds the acetone crystallization, washs, is drying to obtain vinealeucoblastine(VLB) 0.42g, adopt HPLC to detect, its purity is 98.9%.
Embodiment 4
Getting Vinca herb 1Kg, is that 10% acetic acid aqueous solution soaked 2 hours with 10 times of amount concentration, and microwave-assisted extracts, extract power 600W, 4 minutes extraction times, filter, filtrate is regulated pH to 8 with ammoniacal liquor, adopts the absorption of H-103 type macroporous adsorptive resins, with the 50% ethanol elution removal of impurities of pH=5, use 95% ethanol elution again, concentrate eluant adds the acetone crystallization, washs, is drying to obtain vinealeucoblastine(VLB) 0.39g, adopt HPLC to detect, its purity is 97.9%.
Embodiment 5
Getting Vinca herb 1Kg, is that 10% acetic acid aqueous solution soaked 2 hours with 10 times of amount concentration, and microwave-assisted extracts, extract power 600W, 4 minutes extraction times, filter, filtrate is regulated pH to 8 with ammoniacal liquor, adopts the absorption of D-101 type macroporous adsorptive resins, with the 50% ethanol elution removal of impurities of pH=5, use 95% ethanol elution again, concentrate eluant adds the acetone crystallization, washs, is drying to obtain vinealeucoblastine(VLB) 0.37g, adopt HPLC to detect, its purity is 98.4%.
Embodiment 6
Getting Vinca herb 1Kg, is that 10% acetic acid aqueous solution soaked 2 hours with 10 times of amount concentration, and microwave-assisted extracts, extract power 600W, 4 minutes extraction times, filter, filtrate is regulated pH to 8 with ammoniacal liquor, adopts the absorption of DA-201 type macroporous adsorptive resins, with the 50% ethanol elution removal of impurities of pH=5, use 95% ethanol elution again, concentrate eluant adds the acetone crystallization, washs, is drying to obtain vinealeucoblastine(VLB) 0.45g, adopt HPLC to detect, its purity is 98.4%.
Embodiment 7
Getting Vinca herb 1Kg, is that 10% acetic acid aqueous solution soaked 2 hours with 10 times of amount concentration, and microwave-assisted extracts, extract power 600W, 4 minutes extraction times, filter, filtrate is regulated pH to 8 with ammoniacal liquor, adopts the absorption of DS-401 type macroporous adsorptive resins, with the 50% ethanol elution removal of impurities of pH=5, use 95% ethanol elution again, concentrate eluant adds the acetone crystallization, washs, is drying to obtain vinealeucoblastine(VLB) 0.35g, adopt HPLC to detect, its purity is 98.0%.
Embodiment 8
Getting Vinca herb 1Kg, is that 10% acetic acid aqueous solution soaked 2 hours with 10 times of amount concentration, and microwave-assisted extracts, extract power 600W, 4 minutes extraction times, filter, filtrate is regulated pH to 8 with ammoniacal liquor, adopts the absorption of DM-301 type macroporous adsorptive resins, with the 50% ethanol elution removal of impurities of pH=5, use 95% ethanol elution again, concentrate eluant adds the acetone crystallization, washs, is drying to obtain vinealeucoblastine(VLB) 0.39g, adopt HPLC to detect, its purity is 97.9%.
Claims (6)
1, a kind of preparation method of vinealeucoblastine(VLB) is characterized in that described method comprises the following steps: to get the Vinca herb, and doubly measuring concentration with 8-12 is that the acetic acid aqueous solution of 5-20% soaked 2 hours, microwave-assisted extracts, and extracts power 600W, extraction time 2-8 minute, filter, filtrate is regulated pH to 8 with ammoniacal liquor, adopts macroporous adsorptive resins absorption, with the 20-60% ethanol elution removal of impurities of pH=5, use 95% ethanol elution again, concentrate eluant adds the acetone crystallization, washs, is drying to obtain.
2,, it is characterized in that described extraction is 10% with acetic acid aqueous solution concentration according to the preparation method of the described a kind of vinealeucoblastine(VLB) of claim 1.
3,, it is characterized in that described extraction is 10 times of amounts with the acetic acid aqueous solution consumption according to the preparation method of the described a kind of vinealeucoblastine(VLB) of claim 1.
4,, it is characterized in that described microwave-assisted extraction time is preferably 4 minutes according to the preparation method of the described a kind of vinealeucoblastine(VLB) of claim 1.
5, according to the preparation method of the described a kind of vinealeucoblastine(VLB) of claim 1, the model that it is characterized in that described macroporous adsorptive resins is one or more among H-1020, X-5, AB-8, H-103, D-101, DA-201, DS-401, the DM-301.
6, according to the preparation method of the described a kind of vinealeucoblastine(VLB) of claim 1, it is characterized in that described macroporous resin wash-out except that using mixedly alcohol concn is 50%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910027239A CN101643478A (en) | 2009-05-26 | 2009-05-26 | Process for preparing vinblastine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910027239A CN101643478A (en) | 2009-05-26 | 2009-05-26 | Process for preparing vinblastine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101643478A true CN101643478A (en) | 2010-02-10 |
Family
ID=41655561
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910027239A Pending CN101643478A (en) | 2009-05-26 | 2009-05-26 | Process for preparing vinblastine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101643478A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106188055A (en) * | 2016-07-01 | 2016-12-07 | 郑州轻工业学院 | Enzyme auxiliary complexing abstraction is utilized to extract the method separating catharanthine from Herba Catharanthi Rosei |
-
2009
- 2009-05-26 CN CN200910027239A patent/CN101643478A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106188055A (en) * | 2016-07-01 | 2016-12-07 | 郑州轻工业学院 | Enzyme auxiliary complexing abstraction is utilized to extract the method separating catharanthine from Herba Catharanthi Rosei |
| CN106188055B (en) * | 2016-07-01 | 2017-09-15 | 郑州轻工业学院 | The method that complexing abstraction extracts separation catharanthine from catharanthus roseus is aided in using enzyme |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101343305B (en) | Preparation method for astragaloside | |
| CN107362200B (en) | Method for extracting and separating alkaloid and flavone from mulberry leaves | |
| CN102491938B (en) | A kind of purification process of S-GI | |
| CN102453075A (en) | Separation and purification process of glycyrrhizic acid | |
| CN102993154A (en) | Method for extracting purple sweet potato anthocyanin | |
| CN101322737B (en) | Persimmon leaf flavones extract and preparation thereof | |
| CN107722132B (en) | Method for co-producing algal polysaccharide and algal protein from algae | |
| CN101643478A (en) | Process for preparing vinblastine | |
| CN103588849A (en) | Preparation method for glycyrrhetinic acid | |
| CN101602727A (en) | A kind of preparation method of selagine | |
| CN103833805A (en) | Process for refining glycyrrhizinic acid in liquorice | |
| CN112723997A (en) | Green process for extracting high-purity bakuchiol | |
| CN102276515B (en) | Method for extracting deoxynojirimycin | |
| CN112239471A (en) | Method for extracting tetrandrine and tetrandrine | |
| CN111393539A (en) | Preparation method for co-producing tea polysaccharide, theanine and caffeine in summer and autumn tea | |
| CN110960571A (en) | Preparation method of semen astragali complanati total flavonoids | |
| CN109134178A (en) | A method of it is synchronous from watermelon to extract lycopene and citrulling | |
| CN111150765B (en) | Fingered citron flavone extract and separation and purification method thereof | |
| CN110551777A (en) | preparation method of aloe polysaccharide | |
| CN113861248A (en) | Method for treating heavy metals in pomegranate peel extracting solution and purifying punicalagin | |
| CN114031498A (en) | Method for extracting high-purity honeysuckle chlorogenic acid by membrane separation method | |
| CN100364996C (en) | Purification method of catharanthine and vincristine | |
| CN104072463A (en) | Method of extracting quercetin from myricaria | |
| CN104262452A (en) | Method for preparing obakulactone from waste liquid of extracting berberine from phellodendron bark | |
| CN102757429B (en) | Process for producing acehytisine hydrochloride by biologically converting aconitum coreanum hair root |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20100210 |