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Vinblastine extraction and purification method

A purification method, the technology of vinblastine, applied in the direction of organic chemistry, etc., can solve the problems of not being able to meet the use requirements, low vinblastine content, etc., and achieve the effect of less time consumption, increased content and yield, and obvious separation effect

Active Publication Date: 2015-01-07
HAINAN XI YUAN CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But because contain dozens of alkaloids in the periwinkle, vinblastine content is very low, only a few ten-thousandths, and the vinblastine sulfate crude product content after extracting and initial salification is only about 60%, can't meet the use requirement, needs further to it purification

Method used

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  • Vinblastine extraction and purification method
  • Vinblastine extraction and purification method

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Using periwinkle (fresh) as raw material, extract and separate vinblastine sulfate according to the following method:

[0039] 1. Extract the crude product of vinblastine sulfate:

[0040] (1) Take 100kg of periwinkle flowers, add them to 900kg of 20% sodium chloride aqueous solution, soak them in ultrasonic for 15 minutes, then take out the periwinkle flowers and put them directly into cold air at -20°C with a flow rate of 6m / s for 20 minutes. Crush the periwinkle.

[0041] (2) Add the periwinkle treated in step (1) to 500kg of 30% ethanol, adjust the pH to 1.5 with citric acid, reflux extraction for 2 hours, filter the filtrate, adjust the pH of the filtrate to 8-9 with sodium hydroxide, and adjust After pH, apply high pressure to the filtrate and spray it from the top of the extraction tank in the form of a spray at a speed of 200 ml / s. The volume ratio is 4.7:1, the filtrate and the extractant are sprayed into the extraction tank at the same time, and the spraying...

Embodiment 2

[0049] Extract vinblastine sulfate crude product according to the method for embodiment 1, difference is: in step (1), the concentration of sodium chloride aqueous solution is 15%, and cold air velocity is 5m / s, and final gained vinblastine sulfate crude product 10.5g, gets The ratio is 0.105‰, and the content of vinblastine sulfate in the crude product is 81.5%.

Embodiment 3

[0051] Extract vinblastine sulfate crude product according to the method for embodiment 1, difference is: in step (1), the concentration of sodium chloride aqueous solution is 25%, and cold air velocity is 8m / s, and final gained vinblastine sulfate crude product 9.2g, gets The ratio is 0.092‰, and the content of vinblastine sulfate in the crude product is 84.6%.

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Abstract

The invention discloses a vinblastine extraction and purification method which comprises the following steps: carrying out salt immersion and freeze-drying pretreatment on Vinca rosea; carrying out acidic extraction on the pretreated raw material, and adding sulfuric acid to obtain a vinblastine sulfate crude product; and carrying out alkalifying extraction, water washing, silica gel column separation and crystallization on the vinblastine sulfate crude product to obtain the vinblastine pure product. The method has the advantages of simple steps and low time consumption; the Vinca rosea is extracted after pretreatment to remove part of water-soluble pigment impurities in the Vinca rosea and crush the Vinca rosea cell walls, thereby being more beneficial to dissolving out the product. The extraction steps and conditions are selected to enhance the yield and content of the crude product; the extraction reagent, leaching reagent, eluting reagent and crystallizing reagent are selected to enhance the yield and purity of the vinblastine; and the primary crystallization is utilized to obtain the vinblastine pure product, thereby simplifying the purification process and implementing the vinblastine separation and purification more quickly; and the end product has high purity and satisfies the clinical demands.

Description

technical field [0001] The invention relates to a method for extracting, separating and purifying vinblastine from periwinkle flowers, and belongs to the technical field of medicine extraction. Background technique [0002] Periwinkle is an important medicinal plant of the genus Periwinkle in the family Apocynaceae, native to South Asia, East Africa and tropical America. The whole plant of periwinkle can be used as medicine for pain relief, anti-inflammation, sleep, laxative and diuresis. The whole plant is toxic, and if ingested by mistake, it will cause leucopenia, thrombocytopenia, muscle weakness, paralysis of limbs and other symptoms. Periwinkle contains dozens of indole alkaloids, vinblastine is one of them, has anti-cancer effect, and is an anti-tumor drug widely used in clinical practice, with high medicinal value, it is extracted at home and abroad The study of separation has a long history. But because contain dozens of alkaloids in the periwinkle, vinblastine co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D519/04
CPCC07D519/04
Inventor 王洪磊张永明孙中亮
Owner HAINAN XI YUAN CHEM TECH
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