Method for extracting cantharidin

A technology of cantharidin and cantharidin, applied in the direction of organic chemistry, can solve the problem of low yield, achieve the effect of improving purity, shortening production cycle, and increasing yield

Inactive Publication Date: 2007-05-23
芜湖天远生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the extraction process of its cantharidin, the patent first acidifies the cantharidin powder with hydrochloric acid for 24 hours, then cold-soaks it with acetone for 72 hours, and the extraction time is as long as 96 hours. The yield is 0.6%, which is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Extraction process: 100 kg of cantharidin body, dried and crushed into 40-60 mesh, added 1 kg of hydrochloric acid and 300 kg (CP grade) acetone, stirred intermittently and slowly for 5 hours at normal temperature and pressure, then suction filtered, and the The filtered filtrate was distilled and concentrated at 60°C until no liquid flowed out. The evaporated concentrated solution was cooled to room temperature and left for 5 hours; (30°C-60°C) Petroleum ether = 1:1.5 (volume ratio) Wash several times until the washing liquid becomes clear.

[0018] Recrystallization process: the product after washing is fully drained, added 40 times the volume of (AR grade) acetone and refluxed for 20 minutes, filtered while hot, cooled and crystallized naturally, suction filtered after crystallization, and then used 95% weight concentration ethanol: (30 ℃-60 ℃) sherwood oil=1: 1.5 (volume ratio) washing, draining, drying below 60 ℃, obtains 900 grams of cantharidin finished products,...

Embodiment 2

[0020] Extraction process: 100 kg of cantharidin body, dried and crushed into 40-60 mesh, added 2 kg of hydrochloric acid and 400 kg (CP grade) acetone, stirred intermittently and slowly for 6 hours at normal temperature and pressure, then suction filtered, and the The filtered filtrate was distilled and concentrated at 61° C. until no liquid flowed out. The evaporated concentrated solution was cooled to room temperature and left to stand for 6 hours; the concentrated solution that had been left standing was suction-filtered with 96% weight concentration ethanol: (30°C-60°C) Petroleum ether = 1:2 (volume ratio) for multiple washings until the washing liquid becomes clear.

[0021] The recrystallization process is the same as in Example 1.

[0022] The present embodiment obtains 950 grams of cantharidin finished product, and its purity is 99.6%.

Embodiment 3

[0024] Extraction process: 100 kg of cantharidin body, dried and crushed into 40-60 mesh, added 4 kg of hydrochloric acid and 600 kg (CP grade) acetone, stirred intermittently and slowly for 8 hours at normal temperature and pressure, then suction filtered, and the The filtered filtrate was distilled and concentrated at 62° C. until no liquid flowed out. The evaporated concentrated solution was cooled to room temperature and left to stand for 6 hours; the concentrated solution that had been left standing was suction-filtered with 95% weight concentration ethanol: (30°C-60°C) Petroleum ether = 1:1.5 (volume ratio) Wash several times until the washing liquid becomes clear.

[0025] The recrystallization process is the same as in Example 1.

[0026] The present embodiment obtains 960 grams of cantharidin finished product, and its purity is 99.8%.

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Abstract

The invention discloses a method for extracting cantharidin, including extraction and recrystallization process. The said extraction process includes: (1) cold maceration process: drying and meshing mylabris worms into 40-60 meshes, adding maceration solvents and stirring for 5-10 h, and vacuum-filtering at a mylabris worms/hydrochloric acid/acetone weight ratio of 1:0.01-0.05:3-9; (2) concentration and standing process: concentrating and distilling the filtrate at 40-60degreeC until no liquid flows out, cooling to room temperature, and placing for 5-9 hours; and (3) washing process: vacuum-filtering the concentrated liquid, and washing with the mixed solution of ethanol and petroleum ether for several times until the liquid clears up. Compared with the existing technology, this invention has the advantages of simplified process, short production cycles, simple operation, and high yield (increase by 50% compared with the existing technology).

Description

Technical field: [0001] The invention belongs to a method for extracting compounds from animals and plants, in particular to a method for extracting cantharidin from cantharidin bodies. Background technique: [0002] Cantharidin is the earliest anti-cancer drug found in Chinese traditional medicine, and its active ingredient is cantharidin (Cantharidin, C 10 h 12 o 4 ), it has a strong inhibitory and destructive effect on a variety of cancer cells. The preparation method of sodium cantharidinate is disclosed in Chinese patent "preparation process of sodium cantharidate" (publication number: CN1374310), and it comprises the extraction of cantharidin, recrystallization, steps such as preparation sodium cantharidinate. In the extraction process of its cantharidin, the patent first acidifies the cantharidin powder with hydrochloric acid for 24 hours, then cold-soaks it with acetone for 72 hours, and the extraction time is as long as 96 hours. The yield is 0.6%, which is low....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/18
Inventor 唐庆华姚云山唐晓辉
Owner 芜湖天远生物科技有限公司
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