Method for preparing simplified high-purity bulleyaconitine A

A high-purity technology of sulfamethoxine, applied in the direction of organic chemistry and the like, can solve the problems of difficulty in starting raw material sulfamethoxine, high production safety risk, difficult separation and purification of impurities, etc., and achieves shortened production cycle, stable product quality, The effect of low production cost

Inactive Publication Date: 2010-09-15
云南珏草生物科技有限公司
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Problems solved by technology

There are problems such as low content, high production cost, high production safety risk, etc., and it is difficult to industrialize large-scale production
In the patent of CN1054976A, the method of semi-synthesizing aconitine from aconitine is disclosed. In actual ope

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0024] a) extraction

[0025] Take 10KG root tubers of Aconitum aconitum, clean them, soak them in 5L of 1-2% alkali solution for 24-26 hours, take them out, grind them into coarse powder with a diameter of 1-5 mm, heat them with solvent gasoline or petroleum ether 60-90 or n-hexane Reflux extraction five times, each time the weight of the solvent is 5-6 times of the weight of the medicinal material, the first and second extraction reflux times are respectively 2 hours, the third, fourth and fifth extraction reflux times are respectively After 1 hour, 250-300 L of the refluxed extracts were combined, cooled to room temperature, and set aside.

[0026] 2) Column elution

[0027] First put the silica gel into the column, put 250-300L of the extract obtained in step (1) on the column, and use a volume ratio of solvent gasoline: ethyl acetate: triethylamine or diethylamine is 90-95: 1-10: 1-5 : or petroleum ether (60-90): ethyl acetate: triethylamine or diethylamine is 90-95: 1-...

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Abstract

The invention relates to a method for preparing simplified high-purity bulleyaconitine A, which comprises the following steps of: immersing tuberous root of kusnezoff monkshood root in 1 to 2 percent alkaline solution; crushing the tuberous root; performing heat reflux extraction with gasoline or petroleum ether 6 and the like; loading the extract; eluting the tuberous root with solvent gasoline, ethyl acetate and triethylamine or diethylamine in a volume ratio of 90-95 to 1-10 to 1-5; concentrating the eluent under reduced pressure till the eluent is dry; then thermally dissolving the eluent with the solvent gasoline; standing the obtained solution for 20 to 24 hours at normal temperature; crystallizing, filtering and drying the solution to obtain the crude product of the bulleyaconitine A; fully dissolving the crude product in methanol on a water bath of 45 to 55 DEG C; filtering the obtained solution and preserving the heat for 30 minutes on the water bath of 45 to 55 DEG C; adding pure water or distilled water dropwise to assist in the crystallization; standing the solution for 20 to 24 hours at normal temperature to form a crystal; performing filtration to remove the liquid part; washing the crystal for three times; and pumping the crystal and drying the crystal to obtain the finished product. The process has the advantages of simplified production flow, low cost, no three-waste emission, simple operation, high production safety and high extraction rate of the bulleyaconitine A.

Description

technical field [0001] The invention relates to a process method for extracting effective components from Chinese medicinal materials, in particular to a method for extracting aconitin from the tuber root of a kind of plant Aconitum aconitum. technical background [0002] Bulleyaconitione A has a molecular formula of C35H49O10N and a molecular weight of 643.77. It is a colorless prismatic crystal or white powder. Soluble in ether, chloroform, ethanol, dilute acid water, insoluble in water, has strong analgesic and obvious anti-inflammatory effects. Experiments have proved that the analgesic effect of this product is central and closely related to the level of serotonin in the brain. The onset time is slower than that of morphine (37.8 minutes on average), but the maintenance time is longer (9.3 hours on average). Non-addictive. Its anti-inflammatory effect does not pass through the adrenal system, but is related to the suppression of PG levels; this product also has antipy...

Claims

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Application Information

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IPC IPC(8): C07D221/22
Inventor 张红彬
Owner 云南珏草生物科技有限公司
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