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Method for preparing monoester type alkaloids using Chinese medicinal material of aconitum as raw material

A technology of monoester alkaloids and Chinese medicinal materials, applied in the field of natural medicinal chemistry, can solve the problems of easy extraction, slow research progress, unfavorable alkaloid separation and extraction, etc., and achieve the effect of simple method

Active Publication Date: 2008-11-12
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

However, according to experiments, it has been proved that aconitum alkaloids are easy to decompose in methanol, so it is not suitable for large-scale extraction
There are also documents proposing to extract aconitum alkaloids with ethanol extraction (Ding Lisheng, etc., natural product research and development: Vol.6 (3), 1994, 50-54), but ethanol extraction also has its shortcomings, such as: easy Impurities such as starch and polysaccharides are extracted, which brings inconvenience to the subsequent separation work
The separation method of monoester aconitum alkaloids mainly adopts column chromatography at present, but column chromatography has the disadvantage of low yield due to irreversible adsorption, and the separation process is very time-consuming and labor-intensive, which is not conducive to the large-scale separation of alkaloids extract
In summary, although the research on monoester aconitum alkaloids is very urgent, due to the difficulty of separation and extraction, the research progress is slow

Method used

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  • Method for preparing monoester type alkaloids using Chinese medicinal material of aconitum as raw material
  • Method for preparing monoester type alkaloids using Chinese medicinal material of aconitum as raw material
  • Method for preparing monoester type alkaloids using Chinese medicinal material of aconitum as raw material

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Embodiment 1

[0016] Make 500 grams of dried Aconitum aconitum powder and immerse in 95% ethanol by volume concentration for ultrasonic extraction for 2.5 hours, cold soak at room temperature for 24 hours at 20-25°C, the amount of ethanol (ml) is 5 times the weight (g) of the medicinal material powder, Filter out the ethanol extract, treat the dregs soaked twice according to the above method, combine the ethanol extract filtered three times, evaporate the solvent under reduced pressure at 50°C, and obtain a crude extract. Pour 10 times the absolute ethanol of the weight of the crude extract into the crude extract to carry out alcohol precipitation, centrifuge to obtain the filtrate, evaporate the solvent under reduced pressure at 50°C to make the total alkaloid extract; The hexane-ethanol-water system is used for extraction, the volume ratio of the cyclohexane-ethanol-water is 2:1:1, the lower layer solution obtained after the extraction and layering is taken and the solvent is distilled off...

Embodiment 2

[0018] 500 grams of dried Aconitum aconitum powder were immersed in 95% ethanol for ultrasonic extraction for 3 hours, cold soaked at room temperature for 24 hours at 20 to 25°C, and the amount of ethanol (ml) was 5 times that of the medicinal material powder weight (g). Filter out the ethanol extract, treat the dregs soaked twice according to the above method, combine the ethanol extract filtered out three times, and evaporate the solvent under reduced pressure at 55°C to obtain a crude extract. Pour dehydrated ethanol of 11 times the weight of the crude extract into the crude extract to carry out alcohol precipitation, centrifuge to obtain the filtrate, evaporate the solvent under reduced pressure at 55°C to make the total alkaloid extract; The hexane-ethanol-water system is used for extraction, the volume ratio of the cyclohexane-ethanol-water is 2:1:1, the lower layer solution obtained after extraction and layering is taken and the solvent is distilled off under reduced pre...

Embodiment 3

[0020] Soak 500 grams of dried powder of Heishun slices in 95% ethanol for 2 hours, then cold soak at 20-25°C for 24 hours, the amount of ethanol (ml) is 5 times the weight (g) of the medicinal material powder , filter out the ethanol extract, treat the dregs soaked twice according to the above method, combine the ethanol extract filtered out three times, evaporate the solvent under reduced pressure at 65°C, and obtain a crude extract. Pour 12 times the absolute ethanol of the weight of the crude extract into the crude extract to carry out alcohol precipitation, centrifuge to obtain the filtrate, and evaporate the solvent under reduced pressure at 65°C to make the total alkaloid extract; The hexane-ethanol-water system is used for extraction, the volume ratio of the cyclohexane-ethanol-water is 2:1:1, the lower layer solution obtained after the extraction and layering is taken and the solvent is distilled off under reduced pressure at 65°C, Prepare monoester-type alkaloid crud...

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Abstract

The invention provides a method for taking Aconitum Chinese medicine as raw material to prepare mono-ester aconitum alkaloids. The method is as follows: radic aconite kusnezoffii preparata and radix aconiti praeparata of the Aconitum Chinese medicine is quenched by ethanol; alcohol precipitation is performed by anhydrous alcohols and then extraction is performed; extractum is prepared by lower solution and then prepared into alkaline water solution with the pH between 7.5 and 9.5; the solution is placed in a water bath at a temperature of 100 DEG C for 3 hours; chloroform is used for extraction after cooling of the solution; the extracted chloroform solution is evaporated to prepare extractum and then the mono-ester aconitum alkaloids are obtained. The extraction and separation effects are good through electro-spray mass spectrometric detection. The gross production rate of the mono-ester aconitum alkaloids calculated is over 0.21 percent.

Description

technical field [0001] The invention belongs to the field of natural medicinal chemistry, and in particular relates to a method for preparing monoester alkaloids from traditional Chinese medicinal materials of the genus Aconitum, such as Heishun Tablets, Zhichuanwu, Zhicaowu and the like. Background technique [0002] Chinese herbal medicines such as Zhicaowu, Heishunpian and Zhichuanwu are the processed products of the traditional Chinese medicine Fuzi, Chuanwu and Caowu, all of which are commonly used Chinese herbal medicines in clinical practice. The types of alkaloids in the traditional Chinese medicines Aconitum and Aconitum are mainly diester types, and the representative compounds mainly include: aconitine (AC), mesaconitine (MA), hypoaconitine (hypaconitine, HA) It has a wide range of pharmacological activities, such as: anti-inflammatory, analgesic, cardiotonic, anti-myocardial ischemia and hypoxia, etc., but it also has the disadvantages of high toxicity and low to...

Claims

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Application Information

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IPC IPC(8): A61K36/714C07D221/22A61P29/00A61P9/10
Inventor 宋凤瑞包懿刘志强皮子凤刘淑莹
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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