Separation purification process of cantharidin

A technology for separation and purification of cantharidin, applied in the field of separation and purification, can solve the problems of environmental pollution, low yield, high hazard, etc., and achieve the effects of simplified operation steps, high purity and yield, and cost reduction

Inactive Publication Date: 2008-01-23
GUIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main shortcoming of above technology is as follows: (1) in the process of operation, the step of washing consumes a large amount of organic solvents such as ethanol, sherwood oil; The organic solvents such as these wasted ethanol, sherwood oil are higher to the harm of operating personnel simultaneously, and seriously polluted environment
(2) The operation is extensive, and more cantharidin is wasted in the washing process, which is a serious waste of natural resources; the yield is low, resulting in an increase in cost
(3) After recrystallization, there are still more cantharidin and impurities that cannot be separated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Preparation of the crude extract: put the cantharidin body at 60°C and dry it, pulverize it into a powder of about 40 meshes, put it into the reactor, add 3 times the weight of chloroform, shake well, add 2 times the weight distilled water, add hydrochloric acid to adjust the pH = 1, stand still for 48 hours, take out the liquid separation, filter, and concentrate with a rotary evaporator until no liquid flows out to obtain the crude cantharidin extract, which is set aside.

[0014] Put 15g of cantharidin crude extract (cantharidin content is 2.86g after determination) into a container, close the container, let in air, heat until the cantharidin crude extract melts and boils, and the surface temperature of the liquid is about 150°C , a large amount of white smoke in the container is brought into the cooling device by the gas, and white powder is obtained.

[0015] Recrystallization process: Add 80 times the volume of ethyl acetate to dissolve the white powder, heat to r...

Embodiment 2

[0017] Cantharidin crude extract 15g (the measured cantharidin content is 2.86g) is put into the container, closes container, feeds CO 2 , heated to 150°C, the crude cantharidin extract melts, and a large amount of white smoke in the container is brought into the cooling device by the gas to obtain a white powder.

[0018] The recrystallization process is the same as in Example 1.

[0019] In this embodiment, 2.31 g of cantharidin crystals (purity>98%) were obtained, and the yield of cantharidin was 80.87%.

Embodiment 3

[0021] Cantharidin crude extract 15g (cantharidin content is 2.86g after measuring) is put into container, closes container, feeds air, is heated to 140 ℃, and cantharidin crude extract melts, and a large amount of white smog is carried by gas in the container. into a cooling device to obtain a white powder.

[0022] The recrystallization process is the same as in Example 1.

[0023] In this example, 2.23 g of cantharidin crystals (purity>98%) were obtained, and the yield of cantharidin was 77.87%.

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PUM

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Abstract

The invention discloses a cantharidin separation and purification method, which comprises the following steps: (1) the crude extract of the cantharidin is put in a vessel which is sealed, and is connected with air or CO2 and heated to 140 DEG C. to 150 DEG C., the crude extract of the cantharidin is melted and boiled and the large amount of white smog is taken to the cooling device by the air to gain the white power. (2) the ethyl acetate with 80 times volume is added to dissolve the white powder and is heated and refluxed under 80 DEG C. for 10min, and is filtered while heating and is cooled naturally to recrystallize, and conducts pumping filtration, is washed using the volume rate of 1 : 2 between the absolute ethyl alcohol and (30 DEG C. to 60 DEG C.) petroleum ether, and dried under room temperature to gain the cantharidin. The invention is characterized in that the invention has high product purity, high yield, low consumption of the organic solvent and simplified technology.

Description

technical field [0001] The invention belongs to the field of chemical industry, in particular to a separation and purification method. Background technique [0002] Cantharidin is a monoterpenoid defense substance produced by insects of the family Meloidae. The history of human use of cantharidin can be traced back to China in the 1st and 2nd centuries BC. In the ancient medical book "Shen Nong's Materia Medica", there has been a record of medicinal "cantharidin" (insects of the family Corthariaceae). Since then, there have been records about Coriander worm in famous medical books of all dynasties. Modern medicine believes that cantharidin has anti-tumor pharmacological effects, and has significant curative effects on cancers such as liver cancer, laryngeal cancer, cardia cancer, esophageal cancer, and digestive tract tumors, especially for primary liver cancer. In addition to anti-cancer, it also has the functions of treating viral chronic hepatitis B, leukemia, rabies, s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/18
Inventor 李晓飞陈祥盛侯晓晖
Owner GUIZHOU UNIV
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