Preparation method of high purity bulleyaconitine A

A high-purity technology of aconitin, applied in antipyretics, nervous system diseases, organic chemistry, etc., can solve the problems of high production cost, low content, and difficulty in industrialized large-scale production, and achieve low production cost and high product purity High, simple process effect

Active Publication Date: 2009-10-14
KPC PHARM INC
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  • Abstract
  • Description
  • Claims
  • Application Information

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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 operation, it is difficult to separate and purify the impurities produced by the reaction, and it is difficult to separate and obtain qualified starting raw material aconitine, which leads to high production cost and also Difficult to industrialize large-scale production

Method used

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  • Preparation method of high purity bulleyaconitine A
  • Preparation method of high purity bulleyaconitine A

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Get 1kg of Aconiti officinalis root tuber cleanly selected and crushed into coarse powder, use 0.5% hydrochloric acid and 75% methanol aqueous solution as the extraction solvent, soak for 12 hours, and reflux extraction for 3 times, each time for 3 hours, the volume-weight ratio of the amount of extraction solvent to the medicinal material The ratio is 6:1. Concentrate under reduced pressure at 80°C until there is no alcohol, cool to room temperature, make the relative density about 1.10, pH 2.0-3.0, let it stand for 12 hours, and filter to obtain the acidic water extract. Adjust the pH of the obtained acid water extract to 7.0±0.5 with ammonia water, and extract with ethyl acetate whose volume ratio between the acid water liquid and the extraction solvent is 1:3 each time, and extract three times. Concentrate and recover the extraction solvent to obtain an ethyl acetate extraction paste. The obtained extraction paste was eluted with silica gel for column chromatography...

Embodiment 2

[0034] Take 1kg of Aconiti officinalis root tubers and grind them into coarse powder, use 0.7% hydrochloric acid and 95% ethanol aqueous solution as the extraction solvent, soak for 24 to 48 hours, and percolate at a rate of 5ml / min.kg. The ratio of volume to medicinal material weight is 30:1. Concentrate the percolation solution at 80°C under reduced pressure to no alcohol, cool to room temperature, make the relative density 1.10, pH 1.0-3.0, let stand for 18 hours, filter to obtain acid water extract. Adjust the pH of the obtained acid water extract to 7.0±0.5 with 1 mol / L sodium hydroxide aqueous solution, and extract with chloroform with a volume ratio of acid water and extraction solvent of 1:5 each time, and extract 4 times. Concentrate and recover the extraction solvent to obtain a chloroform extraction paste. The obtained extraction paste is eluted with a weight ratio of 1:50 column chromatography with alumina as a filler, and the cyclohexane-acetone-diethylamine syst...

Embodiment 3

[0037] Take 1kg of Aconiti officinalis root tubers, cleanly select and crush them into coarse powder, use 1.0% hydrochloric acid and 75% isopropanol aqueous solution as extraction solvent, soak for 24 to 48 hours, and percolate at a percolation rate of 3ml / min.kg. The ratio of the total volume of the roller to the weight of the medicinal material is 30:1. Concentrate the percolation liquid at 90°C under reduced pressure to no alcohol, cool to room temperature, make the relative density 1.15, pH 1.5-3.0, let stand for 20 hours, filter to obtain acid water extract. The obtained acid water extract was adjusted to pH 8.0 ± 0.5 with 1 mol / L potassium hydroxide aqueous solution, extracted with chloroform each time with a volume ratio of acid water and extraction solvent of 1:4, and extracted 4 times. Concentrate and recover the extraction solvent to obtain an ethyl acetate extraction paste. The obtained extraction paste was eluted with silica gel for column chromatography with a we...

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Abstract

The invention relates to a preparation method of high purity bulleyaconitine A. The preparation method comprises the following steps: root of radix aconiti feri of Yunnan is crushed, and acid alcoholic solvent or alcohol water solution is used for diacolation, and supersound or thermal refluxing extraction. The extracting solution is decompressed and concentrated to be non-alcoholic at the temperature of 80 to 90 DEG C, cooled down to room temperature, to ensure the relative density to be 1.00 to 1.30; standing is performed for 10 to 20 hours; the extracting solution is filtered; the pH is adjusted to 6.0 to 8.0 with basifier; and then the extracting solution is extracted with ethyl acetate or chloroform. The ethyl acetate or chloroform liquid is contracted, column chromatography is performed to the obtained paste, silica gel or neutral alumina are used as fillers, any one of solvent vapor-acetone-diethylamine, ligarine-acetone-diethylamine or cyclohexane-acetone-diethylamine is used for eluation, the bulleyaconitine A in the collected liquid is constantly checked during the thin layer chromatography, the collected liquid containing the bulleyaconitine A is merged, the solvent is concentrated, carbinol or ethanol is dissolved, filtering is performed, crystallization is performed at room temperature, filtering is performed, the crystal is repeatedly rinsed with carbinol or ethanol, and the final product is obtained. The purity of the obtained product is high, the production cost is low, and the toxicity of the used organic solvent is low.

Description

technical field [0001] The invention relates to a method for extracting high-purity aconitin from the root tuber of a kind of natural plant Aconitum aconitifolia. Background technique [0002] Bullyaconitione A (Bulleyaconitione A) was also known as Dianxi doulaine A or dragon head aconitine A, molecular formula C 35 h 49 o 10 N, molecular weight 643.77, is a colorless prismatic crystal. Soluble in ether, alcohol, 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. 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 antipyretic and local anesthetic effects. After taking the medicine, there were no abnormal changes in the patients' ECG, EEG, liver and kidney function and urine routine examinati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D221/22A61P29/00A61P25/04
Inventor 张伟黄照昌朱泽龚云麒
Owner KPC PHARM INC
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