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A high-efficiency extraction and separation method of aconitin

A technology of clathrin and a separation method, which is applied in the field of extraction and separation of clathrate, can solve problems such as unsafe production personnel, high cost, environmental pollution, etc., and achieve the effects of reducing personnel harm, high cost, and reducing environmental pollution.

Active Publication Date: 2016-05-25
云南大围山生物制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because of the use of highly toxic organic solvents benzene and chloroform and a large amount of flammable and explosive organic solvents, it brings unsafe factors to production personnel, and the cost is high, and it also inevitably causes environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Pre-treatment: take 500 g of Aconitum aconitum root, sort it, remove impurities, and crush it into coarse powder.

[0023] (2) Extraction and concentration: take the coarse powder of Aconitum aconitum medicinal material, put it in a round bottom flask, add acidic 75% ethanol solution containing 3‰ mass fraction of sulfuric acid to extract three times, and extract for the first time: add The acidic 75% ethanol solution containing 3‰ of sulfuric acid, which is 3.2 times the weight of the coarse powder of Aconitum aconitum, is controlled at a steam pressure of 0.1 MPa, heated to 60°C for 12 hours, filtered, and the filtrate is collected; the second and third times use In the same method as the first time, add the acid 75% ethanol solution containing sulfuric acid 3‰ described in the filter residue of 2.4 times weight respectively in each filter residue, extract respectively 2 hours (extract 2 hours for the second time), extract 4 hours (extract 4 hours for the second t...

Embodiment 2

[0029] Embodiment 2 Except that the operations of the following steps are different, the operations of the remaining steps are the same as those of Embodiment 1, and will not be repeated here.

[0030](2) Leaching and concentration: the combined extract was filtered and concentrated in a vacuum at 0.04 MPa to recover to no alcohol smell, and the concentrated solution was diluted with purified water 1.5 times the weight of the concentrated solution to a relative density of 1.07.

[0031] (4) Extraction: inject the alkalized filtrate of step (3) into a separatory funnel, add ethyl acetate whose volume is twice the volume of the alkalized filtrate, stir and extract for 45 minutes, and let stand for 3 hours.

[0032] Concentrate the combined ethyl acetate extracts in a vacuum at 0.04MPa, control the temperature at 65°C, concentrate and recover the ethyl acetate to a thick paste, collect the thick paste, put it into a clean container, and weigh it.

[0033] The obtained total alkal...

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PUM

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Abstract

A bulleyaconitine A efficient extraction and separation method comprises pretreatment, extraction, concentration, acidification, basification, extraction, column chromatography and crystallization steps. According to the method, 75% acid ethanol solution containing 0.3% of sulfuric acid is used for extraction for three times, concentrated ammonia water is slowly added under stirring during alkalization to adjust pH to 8, loss of bulleyaconitine A is reduced; during column chromatography on silica gel, the flow rate of the column chromatography is reasonably and effectively controlled at 13-20ml / min, the separation effect is better; ethyl acetate is used for extraction, the solvent residue is zero, the bulleyaconitine A highest content can reach 98-99%, the product purity is high, and the rate extraction of the bulleyaconitine A of a radix aconiti kusnezoffii medicinal material can be increased to 0.15 to 0.22 %. The method uses non-toxic or low-toxic organic solvents and reduces organic solvent kinds and usage amount, saves energy, reduces conservation, and reduces personnel hazards and environmental pollution.

Description

technical field [0001] The invention belongs to the technical field of extracting, separating and purifying active ingredients of plants, and in particular relates to an industrialized technology for extracting and separating aconitin from raw medicinal materials of Aconitum aconitum. Background technique [0002] In recent years, the alkaloid Bulleaconitine A isolated from the herbal medicine Dianxi Aconitum used for analgesic and anti-inflammatory in western Yunnan, also known as Dianxi Duraconitine A, is an excellent analgesic and anti-inflammatory drug , its analgesic effect is stronger than aconitine, and its immunomodulatory effect is weaker than aconitine. It has dual pharmacological effects of central analgesia and peripheral analgesia. Aconitin is suitable for the treatment of advanced cancer pain, rheumatic and rheumatoid arthritis, frozen shoulder, shoulder and arm pain, stiff neck, osteoarthritis, benign joint pain, waist and limb joint sprains, contusions, lumb...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D221/22
CPCC07D221/22
Inventor 姜学锋丁燕龙杨福荣武逵唐合柱
Owner 云南大围山生物制药有限公司
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