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Bulleyaconitine A preparation method

A technology of clathrin and aconitum, applied in the field of preparation of clathrate, can solve the problems of complex method steps, difficult preparation, changes, etc., and achieve the effects of being convenient for recycling, improving working environment, and reducing environmental pollution.

Inactive Publication Date: 2016-10-12
YUNNAN UNIV OF TRADITIONAL CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The research results show that its solubility in water is small (166.78μg / mL) and unstable, and it is prone to degradation at room temperature, while its solubility and stability increase with the decrease of pH value, making it difficult to prepare
[0004] Chinese Invention Patent Authorization Announcement No. CN 101555227 B discloses a method for preparing high-purity aconitin by acid alcohol extraction. The chromatographic material used in the purification step of the method is silica gel (200-300 mesh), and the consumption Large and costly; the eluent is a ternary system of petroleum ether / cyclohexane-acetone-diethylamine, the polarity of the solvent changes after recovery, it is not easy to recycle, the cost is high and the method steps are complicated

Method used

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  • Bulleyaconitine A preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] S1. Material selection: select dried Aconitum tuber in western Yunnan, crush it to 50-100 mesh, and set aside;

[0026] S2. Extraction: soak the root tubers of Aconitum aconitum obtained in step S1 with 95% ethanol for 18 hours, then use 8 times the amount of ethanol to extract it for 5 times, combine the leachate, concentrate to a paste, and obtain an extract;

[0027] S3. Extraction and separation: dissolve the extract obtained in step S1 with 1.5% hydrochloric acid, filter to obtain an acid solution, adjust its pH to 10 with 25% concentrated ammonia water, then add 1 volume times of ethyl acetate, and vibrate for 30 -45min, stand for separation, take the supernatant, repeat the extraction 3 times, combine the extracts, recover under reduced pressure to a paste, and obtain the crude total alkali;

[0028] S4. Separation and purification by column chromatography: dissolve the crude total alkali obtained in step S2 with chloroform, and adsorb on 2 times the amount of si...

Embodiment 2

[0031] S1. Material selection: select dried Aconitum tuber in western Yunnan, crush it to 50-100 mesh, and set aside;

[0032] S2. Extraction: soak the root tubers of Aconitum aconitum obtained in step S1 with 95% ethanol for 16 hours, then extract it three times with 10 times the amount of ethanol, combine the leachate, concentrate to a paste, and obtain an extract;

[0033] S3. Extraction and separation: dissolve the extract obtained in step S1 with 1.5% hydrochloric acid, filter to obtain an acid solution, adjust its pH to 10 with 25% concentrated ammonia water, then add 2 volume times of ethyl acetate, and vibrate for 30 -45min, stand for separation, take the supernatant, repeat the extraction 4 times, combine the extracts, recover under reduced pressure to a paste, and obtain the crude total alkali;

[0034] S4. Separation and purification by column chromatography: dissolve the crude total alkali obtained in step S2 with chloroform, and adsorb on 1 times the amount of sil...

Embodiment 3

[0037] S1. Material selection: select dried Aconitum tuber in western Yunnan, crush it to 50-100 mesh, and set aside;

[0038] S2. Extraction: Soak the root tubers of Aconitum aconitum obtained in step S1 with 95% ethanol for 820 hours, then use 9 times the amount of ethanol to extract it 4 times, combine the leachate, concentrate to a paste, and obtain an extract;

[0039] S3. Extraction and separation: dissolve the extract obtained in step S1 with 1.5% hydrochloric acid, filter to obtain an acid solution, adjust its pH to 10 with 25% concentrated ammonia water, then add 2 volume times of ethyl acetate, and vibrate for 30 -45min, stand for separation, take the supernatant, repeat the extraction 3 times, combine the extracts, recover under reduced pressure to a paste, and obtain the crude total alkali;

[0040] S4. Separation and purification by column chromatography: dissolve the crude total alkali obtained in step S2 with chloroform, and adsorb on 2 times the amount of silic...

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Abstract

The invention relates to the natural medicine preparation field, and in particular, relates to a bulleyaconitine A preparation method; the preparation method comprises four steps: extraction, extraction separation, column chromatography separation purification, and crystallization purification. According to the bulleyaconitine A preparation method provided by the invention, alumina column chromatography is used for replacing silica gel column chromatography, so that the production cost is saved; a petroleum ether-diethylamine binary system is used as an eluent and is easy to recycle and reuse, so as to reduce environmental pollution.

Description

technical field [0001] The invention relates to the field of natural medicine preparation, in particular to a preparation method of aconitin. Background technique [0002] Aconitum aconitum and aconite are traditional Chinese medicinal materials in the Ranunculaceae family, and are commonly used in the treatment of rheumatism, rheumatoid arthritis, sciatica and other emergencies. Its water decoction has been used to relieve the pain of patients with advanced tumors. Aconitin is one of its main active ingredients, which has dual pharmacological effects of central analgesia and peripheral analgesia, and has the characteristics of long analgesic time and no addiction. Its side effects are small, it has no obvious damage to vital organs, and it has no teratogenic effect. At present, it is mainly used in the treatment of acute and chronic pain diseases such as herpes zoster and advanced cancer pain, rheumatism and rheumatoid arthritis, frozen shoulder, and benign joint pain. tr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D221/22
CPCC07D221/22
Inventor 左爱学张建英沈勇
Owner YUNNAN UNIV OF TRADITIONAL CHINESE MEDICINE
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