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Catharanthine tartrate preparation method

A technology of vinblastine and tartrate, applied in the direction of organic chemistry and the like, can solve the problems of being unsuitable for industrial production, low vinblastine yield, complicated purification steps and the like, and achieves high product yield, rapid dissolution and high purity. Effect

Inactive Publication Date: 2015-02-25
HAINAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has cumbersome purification steps, long time-consuming, low yield of vinblastine, and is not suitable for industrial production

Method used

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Examples

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Effect test

Embodiment 1

[0047]Using fresh whole plant periwinkle (including root) as raw material, prepare vinblastine tartrate according to the following method:

[0048] 1. Extraction and preparation of crude vinblastine:

[0049] (1) Take 100kg of the whole periwinkle plant, add it to 850kg of 5wt% sodium chloride aqueous solution, soak it in ultrasonic for 15 minutes, then take out the periwinkle and put it directly into the cold air with a flow rate of 6.5m / s at -20°C for 40 minutes to freeze-dry. The periwinkle was crushed after freeze-drying.

[0050] (2) Add the periwinkle treated in step (1) to 300kg of water, adjust the pH to 1.5 with phosphoric acid, soak in ultrasonic for 3 hours, filter to get the filtrate, adjust the pH of the filtrate to 8-9 with ammonia water, after adjusting the pH, put the filtrate Apply high pressure and spray it from the top of the extraction tank in the form of a spray at a speed of 180 ml / s. At the same time, apply high pressure to the extractant and spray it i...

Embodiment 2

[0059] 1. Extraction and preparation of crude vinblastine:

[0060] Extract the crude vinblastine according to the method of Example 1, the difference is: the volume ratio of the filtrate to the extractant in step (2) is 5.5:1, and the extractant is n-bromopropane and ethanol with a volume ratio of 10:0.5 The mixture; in step (4), the volume ratio of dichloromethane and ethyl acetate is 10:3, and the volume ratio of toluene and petroleum ether is 8:1. The mass of the obtained crude vinblastine was 43.2 g, the yield was 0.432‰, and the purity by HPLC was 73.6%.

[0061] 2. Preliminary salt formation of vinblastine:

[0062] 43.2g of crude vinblastine was completely dissolved in 54.5ml of anhydrous methanol to form A solution. 14.1g of tartaric acid was completely dissolved by heating with 54.5ml of anhydrous methanol to form B solution. Slowly add solution B to solution A at 45-50°C, stir evenly after adding, and ultrasonicate at room temperature for 5 minutes. After crystal...

Embodiment 3

[0066] Vinblastine tartrate is prepared according to the method of Example 1, the difference is: when vinblastine tartrate is refined, 50.5g of vinblastine tartrate is added to 202ml of N,N-dimethylformamide solution and heated and stirred until Completely dissolve, then slowly add 202ml of a mixture of anhydrous methanol and ethyl acetate (anhydrous methanol: ethyl acetate volume ratio = 95:5) into the vinblastine tartrate solution, ultrasonicate for 5 minutes, and wait for crystals to form Afterwards, let stand at -18°C for 24 hours, and crystallize. The obtained crystals were suction-filtered at -18°C and freeze-dried at -20°C to obtain 44.8 g of high-purity vinblastine tartrate. The purity was 99.5% by HPLC.

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Abstract

The invention discloses a catharanthine tartrate preparation method. The catharanthine tartrate preparation method includes the steps of subjecting whole catharanthus roseus to brining, freeze drying and smashing; adding powder into water, regulating pH (potential of hydrogen) prior to extraction, and regulating pH of an extracted product to obtain a catharanthine crude product; enabling the catharanthine crude product to react with tartaric acid to salify, and crystallizing in mixed solvents to obtain catharanthine tartrate. The catharanthine tartrate preparation method has the advantages that the method is concise in step, less in consumed time and rapid in product dissolution, the catharanthine crude product high in purity is obtained directly by pH gradient separation with column chromatography separation not required, and the catharanthine tartrate which has the purity above 99% and is easy to preserve can be obtained by salifying and crystallizing; the method is simpler in purification process and capable of realizing separation and purification of catharanthine more rapidly, and the finally obtained product is high in yield and purity and can better satisfy market demand.

Description

technical field [0001] The invention relates to a method for preparing vinblastine tartrate, in particular to a method for preparing vinblastine by using periwinkle as a raw material, 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. The whole plant of periwinkle, especially the root, contains a variety of indole alkaloids, which have good medicinal value. Vinblastine (Catharanthine in English) is one of the vinca alkaloids. Animal experiments have shown that it has antihypertensive effects. It is one of the important ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/22
CPCC07D471/22
Inventor 王洪磊周雪晴张永明窦智峰张名楠孙芳
Owner HAINAN UNIVERSITY
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