Purification method of yunaconitine

A purification method, the technology of yunnanjing, which is applied in the fields of organic chemistry and bulk chemical production, can solve the problems of poor process specificity and achieve the effects of high reproducibility, easy scale-up production, and simple operation

Inactive Publication Date: 2012-07-04
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Such as "Supercritical CO of the total alkaloids of Aconitum 2 Extraction and content determ

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Get Aconitum aconitum medicinal material, pulverize 80 meshes, take 1kg and add 500ml 90% methanol to infiltrate for 2 hours, add in the extraction kettle, open the equipment adjustment parameters: the extraction temperature is 50°C, the extraction pressure is 35MPa, the temperature of the separation kettle 1 is 60°C, The pressure is 10MPa, the temperature of the separation tank II is 40°C, and the pressure is 6MPa. After reaching the above parameters, extract and extract at a flow rate of 30L / h for 2 hours, collect and analyze the extract, dissolve the extract with 4% hydrochloric acid, filter and add 732 strong acidic cation exchange resin for adsorption, take 5BV80% methanol solution (adjust pH9 with ammonia water) , eluted, the eluate was concentrated under reduced pressure without alcohol, added 2BV dichloromethane to extract 3 times, the organic layer was collected and the extract was concentrated, added 100g of neutral alumina to dry (200-300 mesh), packed into a ...

Embodiment 2

[0021] Get Aconitum aconitum medicinal material, pulverize 20 orders, get 1kg and add 500ml 95% ethanol to infiltrate for 2 hours, add in the extraction kettle, open equipment adjustment parameter: extraction temperature is 50 ℃, and extraction pressure is 30MPa, and separation kettle 1 temperature is 50 ℃, The pressure is 8MPa, the temperature of the separation tank II is 35°C, and the pressure is 5MPa. After reaching the above parameters, extract and extract at a flow rate of 35L / h for 2h, collect and analyze the extract, dissolve the extract with 2% hydrochloric acid, filter and add D151 weakly acidic cation exchange resin for adsorption, take 6BV60% ethanol solution (adjust pH 11 with ammonia water) , elution, the eluate was concentrated under reduced pressure without alcohol, added 3BV of dichloromethane to extract twice, collected the organic layer extract and concentrated, added 80g of neutral alumina to dry (200-300 mesh), packed into a column, and used petroleum ether-...

Embodiment 3

[0023] Get the Aconitum aconitum medicinal material, pulverize 60 orders, get 2kg and add 800ml 99% methanol to infiltrate for 1 hour, add in the extraction kettle, open the equipment adjustment parameters: the extraction temperature is 45°C, the extraction pressure is 35MPa, the temperature of the separation kettle 1 is 55°C, The pressure is 9MPa, the temperature of the separation tank II is 35°C, and the pressure is 5MPa. After reaching the above parameters, extract and extract with a flow rate of 38L / h for 2h, collect and analyze the extract, dissolve the extract with 1% hydrochloric acid, filter and add 001×3 strong acidic cation exchange resin for adsorption, take 5BV70% ethanol solution (adjusted with ammonia water) pH10), elution, the eluate was concentrated under reduced pressure without alcohol, added 4BV dichloromethane to extract twice, collected the organic layer extract and concentrated, added 180g of neutral alumina to dry (200-300 mesh), packed into a column, and...

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Abstract

The invention provides a purification method of yunaconitine, which includes the following steps: taking a vilmorrianine medicinal material as the raw material, smashing, adding alcohol, infiltrating for 1 to 2 hours, transferring to an extraction kettle, using supercritical carbon dioxide for extraction, collecting yunaconitine extract, dissolving with acid water, filtering, adding cation exchange resin for absorption, adding alkaline alcoholic solution for elution, enabling eluent to be decompressed and concentrated, adding methylene dichloride for extraction, enabling extract liquor to be concentrated, adding aluminum oxide and packing columns after drying, using petroleum ether methylene dichloride mixed solution for elution, detecting in thin layers, collecting yunaconitine flow content, enabling eluent to be concentrated and placed in small size for crystallization, drying crystals and obtaining the yunaconitine product. The purification method of yunaconitine causes little pollution, and is low in energy consumption, high in yield and suitable for industrial production.

Description

Technical field: [0001] The present invention relates to a kind of purification method of aconitine, in particular to a method of using supercritical CO 2 A method for extracting and purifying aconitine. Background technique: [0002] Dianconitine, also known as isoaconitine and aconitine B, is a diterpene alkaloid with molecular formula C 35 h 49 o 11 , molecular weight 659.77, melting point 142°C-143°C, soluble in methanol and ethanol solutions, easily soluble in acetone, chloroform, dichloromethane and acid water, insoluble in petroleum ether and water. [0003] Dianconitine has anti-inflammatory, analgesic and local anesthetic effects. However, its toxicity is relatively high, and its molecular structure is often modified to reduce toxicity, so it can be used as a raw material for the synthesis of aconitine. The patent "Method for preparing aconitine" and the document "Structure modification of aconitine" both use aconitine as a raw material for structural modificat...

Claims

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Application Information

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IPC IPC(8): C07D221/20
CPCY02P20/54
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司
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