Novel method for extracting vincaleukoblastinum from catharanthus roseus

A technology for vinblastine and vinblastine, which is applied in the field of extracting vinblastine and utilizing the combination of biological enzymes and dual-frequency ultrasonic waves to extract vinblastine, can solve the problems of destroying thermally unstable components, affecting the extraction of vinblastine, and low extraction efficiency, and achieving The effect of low cost, high extraction rate and high extraction rate

Inactive Publication Date: 2014-12-24
NANJING BIAOKE BIO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the extraction methods of vinblastine mainly include traditional Chinese medicine extraction methods such as soaking method, percolation method and reflux method, but the extraction efficiency of these methods is low and the operation is cumbersome.
In rec

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Remove impurities from periwinkle and pulverize them, pass through a 50-mesh sieve, take 500g of powder, add 8 times of 70% ethanol solution, add sulfuric acid to adjust pH to 2.0, add 0.02% of periwinkle weight biological enzyme (cellulase: Hemicellulase: pectinase (0.5:0.2:0.3), put it into a dual-frequency ultrasonic device, the ultrasonic frequency is 20Hz, 40Hz, and the ultrasonic power is 300W, enzymolysis at 40°C for 5h, the enzymatic solution is filtered, and the filtrate Adjust the pH to 10.0 with concentrated ammonia water, extract with ethyl acetate, collect the organic phase, dry over anhydrous sodium sulfate, filter, concentrate under reduced pressure to dryness, dissolve the concentrate in a small amount of ethanol, and perform silica gel column chromatography to obtain methane) and V (methanol) as 18:1 eluent for purification, the eluate was collected and concentrated to obtain 0.18 g of vinblastine with a purity of 96.1%.

Embodiment 2

[0018] Remove impurities from periwinkle and pulverize them, pass through a 50-mesh sieve, take 500g of powder, add 6 times of 80% ethanol solution, add sulfuric acid to adjust pH to 2.5, add 0.04% of periwinkle weight biological enzyme (cellulase: Hemicellulase: pectinase (0.5:0.2:0.3), put it into a dual-frequency ultrasonic device, the ultrasonic frequency is 20Hz, 40Hz, the ultrasonic power is 400W, enzymolysis at 45°C for 6h, the enzymatic solution is filtered, and the filtrate Adjust the pH to 10.0 with concentrated ammonia water, extract with ethyl acetate, collect the organic phase, dry over anhydrous sodium sulfate, filter, concentrate under reduced pressure to dryness, dissolve the concentrate in a small amount of ethanol, and perform silica gel column chromatography to obtain methane) and V (methanol) as 18:1 eluent for purification, the eluate was collected and concentrated to obtain 0.24 g of vinblastine with a purity of 98.8%.

Embodiment 3

[0020] Remove impurities from periwinkle and pulverize them, pass through a 50-mesh sieve, take 500g of powder, add 5 times of 75% ethanol solution, add sulfuric acid to adjust the pH to 3.0, add 0.05% of the weight of periwinkle biological enzyme (cellulase: Hemicellulase: pectinase (0.5:0.2:0.3), put it into a dual-frequency ultrasonic device, the ultrasonic frequency is 20Hz, 40Hz, and the ultrasonic power is 350W, enzymolysis at 50°C for 5.5h, the enzymolysis solution is filtered, The filtrate was adjusted to pH 10.0 with concentrated ammonia water, extracted with ethyl acetate, the organic phase was collected, dried over anhydrous sodium sulfate, filtered, concentrated to dryness under reduced pressure, dissolved in a small amount of ethanol, subjected to silica gel column chromatography, and extracted with V (di Chloromethane) and V (methanol) as 18:1 eluent for purification, the eluate was collected and concentrated to obtain 0.19 g of vinblastine with a purity of 97.5%....

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Abstract

The invention relates to a novel method for extracting vincaleukoblastinum from catharanthus roseus. The novel method comprises the following steps: removing impurities in catharanthus roseus, crushing, screening by using a 50-mesh sieve, adding an ethanol solution, adding acid to adjust the PH value to be 2-3, adding a biological enzyme after one hour, performing enzymolysis in a double-frequency ultrasonic device, filtering, adjusting the PH value of the filtrate to be 10.0 by using concentrated ammonia water, extracting with ethyl acetate, collecting an organic phase, drying with anhydrous sodium sulfate, filtering, performing vacuum concentration till the materials are dried, dissolving with a small amount of ethanol, and purifying in a silica gel column chromatography manner, thereby obtaining the high-purity vincaleukoblastinum. The novel method has the advantages of simple process, high extraction rate and high product purity, and is applicable to industrialization production.

Description

technical field [0001] The invention relates to a new method for extracting vinblastine from vinca flowers, in particular to a method for extracting vinblastine by combining biological enzymes and dual-frequency ultrasonic waves, and belongs to the technical field of natural medicines. Background technique [0002] Periwinkle, also known as Yanlaihong, Ririxin, Four Seasons Spring, and Sanwanhua, is the whole herb of the Apocynaceae periwinkle. Vinca contains a large amount of alkaloids with complex structure, poor thermal stability, and the content is very small. Vinblastine is the most important one among them. It is needle-like crystal, insoluble in water and petroleum ether, soluble in ethanol, acetone, ethyl acetate, chloroform, methanol, bitter in taste, hygroscopic, and gradually turns yellow when exposed to light or heat. , mp211 ~ 216 ℃, with anti-tumor activity, can be used for the treatment of Hodgkin's disease and choriocarcinoma, lymphosarcoma and ovarian cance...

Claims

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Application Information

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IPC IPC(8): C07D519/04
CPCC07D519/04
Inventor 张金芳杨存
Owner NANJING BIAOKE BIO TECH
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