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Method for preparing cantharidin from cantharides

A technology of cantharidin and cantharidin, which is applied in the field of cantharidin preparation by supercritical CO2 extraction technology, can solve the problems of low extraction efficiency of active ingredients, high toxicity of cantharidin, long cycle, etc., and achieve high product yield, small amount of solvent, good properties stable effect

Inactive Publication Date: 2010-08-11
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In short, these methods have low extraction efficiency of active ingredients, high reagent consumption, and long cycle time.
And mylabris itself is very toxic, acetone ethyl acetate is volatile, and the operation requirements are very strict.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Get 5 kilograms of cantharidin (cantharidin content 1.1%) and pulverize 20 orders, pack into extraction tower, add 200mlpH earlier and be the acetone of 2 and soak for 1 hour, seal, extraction temperature is adjusted to 30 ℃, separation tower temperature is adjusted to 40 ℃, The extraction pressure is 10MPa, the analytical pressure is 4MPa, CO 2 The gas is released from the steel cylinder, cooled to 0-5°C in the liquefaction tank after passing through the gas purifier, and liquefied. into the storage tank with a high-pressure metering pump to CO 2 and 500ml of acetone into the preheater, through the preheater to the specified temperature and pressure, the acetone is entrained from the lower part of the extraction tower and enters into contact with the material. to 4MPa, open the pressure regulating valve, control the above parameters through the pressure regulating valve, and extract dynamically for 3 hours. Release the extract after shutdown, collect the extract, rec...

Embodiment 2

[0027] Get 5 kilograms of cantharidin (cantharidin content 1.1%) and pulverize 10 orders, pack into extraction tower, add 150mlpH earlier and be the acetone of 3 and soak for 1.5 hours, seal, extraction temperature is adjusted to 40 ℃, separation tower temperature is adjusted to 50 ℃, The extraction pressure is 20MPa, the analytical pressure is 8MPa, CO 2 The gas is released from the steel cylinder, cooled to 0-5°C in the liquefaction tank after passing through the gas purifier, and liquefied. into the storage tank with a high-pressure metering pump to CO 2 and 1000ml of acetone into the preheater, through the preheater to the specified temperature and pressure, the acetone is entrained from the lower part of the extraction tower and enters into contact with the material, the flow rate is 1L / min, and the pressure inside the tower is adjusted. When the extraction pressure reaches 20MPa, the analytical pressure reaches 8MPa , open the pressure regulating valve, control the abov...

Embodiment 3

[0029] Get 5 kilograms of cantharidin (cantharidin content 1%) and pulverize 20 orders, pack into extraction tower, add 200mlpH earlier and be the acetone of 2 and soak for 1 hour, seal, extraction temperature is adjusted to 30 ℃, separation tower temperature is adjusted to 50 ℃, The extraction pressure is 15MPa, the analytical pressure is 6MPa, CO 2 The gas is released from the steel cylinder, cooled to 0-5°C in the liquefaction tank after passing through the gas purifier, and liquefied. into the storage tank with a high-pressure metering pump to CO 2 and 500ml of acetone into the preheater, through the preheater to the specified temperature and pressure, the acetone is entrained from the lower part of the extraction tower and enters into contact with the material, the flow rate is 0.8L / min, and the pressure inside the tower is adjusted. When the extraction pressure reaches 15MPa, the analytical pressure reaches 6MPa, open the pressure regulating valve, control the above par...

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PUM

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Abstract

The invention provides a novel process for preparing cantharidin from cantharides. The process comprises the following steps of: by using supercritical CO2 as a solvent and acetone as an entrainer, performing static immersion of the cantharides for 1 to 1.5 hours at an extraction pressure of 10 to 20MPa and an extraction temperature of between 30 and 40 DEG C, performing dynamic extraction for 2 to 3 hours at an analytic pressure of 4 to 8MPa and an analytic temperature of between 40 and 50 DEG C, removing impurities from the obtained extracts by using petroleum ether, and crystallizing the obtained extracts by using acetone. The process has the advantages of high extraction efficiency, short period, little pollution and low cost.

Description

Technical field: [0001] The present invention relates to a kind of method that prepares cantharidin from cantharidin, especially a kind of method that adopts supercritical CO 2 A method for preparing cantharidin by extraction technology. Background technique: [0002] Cantharidin is a natural monoterpenoid insect toxin present in insects such as Coleopera (Coleopera) and Meloidae (Meloidae), and is a defensive substance in the cantharidin. In 1810, the French pharmacist Robiquet extracted the crude extract of cantharidin for the first time from the Spanish green turnip Lytta vesicatoria. [0003] Chemical structure: exo type, 1,2 cis-dimethyl, 3,6-oxo-hexahydrophthalic anhydride. [0004] Molecular formula and molecular weight: C 10 h 12 o 4 , 196.21. [0005] Physical and chemical properties: insoluble in cold water, hardly soluble in ether (1g / 700ml), solubility in chloroform, dichloromethane, acetone, ethyl acetate (2°C) is 1 / 60, 1 / 80, 1 / 90, 1 / 150 (g / ml). The rec...

Claims

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Application Information

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IPC IPC(8): C07D493/18
CPCY02P20/54
Inventor 刘东锋张翼杨成东
Owner NANJING ZELANG MEDICAL TECH
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