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Preparation method of cynandione A

A technology of uranone and Baishouwu, which is applied in the field of natural medicinal chemistry, can solve the problems of cumbersome method of diketone A, complex components of Baishouwu, and difficulty in industrialized production, etc., and achieves simple and feasible method, easy industrial production, The effect of less impurity dissolution

Inactive Publication Date: 2012-06-27
江苏博益生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Due to the complexity of ingredients in Radix Polygoni Multiflori, the existing methods for preparing Radix Polygonum A are cumbersome and difficult to industrialize

Method used

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  • Preparation method of cynandione A

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Dry and pulverize Baishouwu to 80 meshes, take 2kg and put it into a supercritical extraction kettle, set the extraction pressure to 20MPa, the temperature to 40°C, and feed liquid CO2 at 20kg / h. After the above parameters are reached, feed 90% ethanol solution at 2kg / h to make Entrainer, dynamic extraction for 3 hours, analyze the extract under the conditions of pressure 6MPa and temperature 50°C, add 100g of polyamide resin to the obtained extract to dry, crush the dried product and pack it into a column, take 500ml of 60% ethanol solution to precipitate impurities, and then take 400ml of 90% ethanol Precipitate the target component, concentrate the eluent under reduced pressure to about 50ml, transfer it to a separatory funnel, add an equal volume of chloroform for extraction 3 times, concentrate the extract to about 30ml, place the crystals, filter out the crystals, reflow with absolute ethanol to dissolve the recrystallization, and dry The light yellow crystal radix...

Embodiment 2

[0020] Dry and pulverize Baishouwu to 40 meshes, take 4kg and put it into a supercritical extraction kettle, set the extraction pressure to 30MPa, the temperature to 45°C, and feed liquid CO2 at 25kg / h. After reaching the above parameters, feed 99% methanol solution at 4kg / h to make Entrainer, dynamic extraction for 3 hours, analyze the extract under the conditions of pressure 7MPa and temperature 60°C, add 200g of polyamide resin to the obtained extract to dry, crush the dried product and pack it into a column, take 1200ml of 50% ethanol solution to remove impurities, and then take 1200ml of 80% ethanol Elute the target component, concentrate the eluent under reduced pressure to about 150ml, transfer it to a separatory funnel, add an equal volume of chloroform for extraction twice, concentrate the extract to about 80ml, place the crystals, filter out the crystals, and then reflux with absolute ethanol to dissolve and recrystallize. Dried to obtain pale yellow crystal diketone ...

Embodiment 3

[0022] Dry and pulverize Baishouwu to 60 meshes, take 4kg and put it into a supercritical extraction kettle, set the extraction pressure to 25MPa, the temperature to 50°C, and feed liquid CO2 at 20kg / h. After reaching the above parameters, feed anhydrous acetone solution at 3kg / h for Entrainer, dynamic extraction for 3 hours, analyze the extract under the conditions of pressure 10MPa and temperature 50°C, add 200g of polyamide resin to the obtained extract to dry, crush the dried product into a column, take 1000ml of 60% ethanol solution to remove impurities, and then take 600ml of 99% ethanol Precipitate the target component, concentrate the eluent under reduced pressure to about 120ml, transfer it to a separatory funnel, add an equal volume of chloroform for extraction 3 times, concentrate the extract to about 70ml, place the crystals, filter the crystals, reflow with absolute ethanol to dissolve the recrystallization, and dry The light yellow crystal radix diketone A was obt...

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Abstract

The invention discloses a preparation method of cynandione A. The preparation method of cynandione A comprises the following steps of drying bunge auriculate roots, crushing the dried bunge auriculate roots into powder of 20 to 80 meshes, putting the powder into a supercritical extraction kettle, feeding liquid CO2 and an entrainer into the supercritical extraction kettle, carrying out extraction at a temperature of 40 to 50 DEG C under the pressure of 15 to 30MPa for 2 to 3 hours, carrying out analysis of extract at a temperature of 50 to 60 DEG C under the pressure of 5 to 10MPa, adding the extract obtained by the previous step into polyamide resin, drying, carrying out column packing, carrying out gradient elution by an ethanol solution, collecting eluate, carrying out reduced pressure concentration, carrying out extraction of concentrate obtained by the previous step by chloroform, concentrating extract to a small volume so that crystals are precipitated, carrying out recrystallization of the crystals by absolute ethanol, and drying to obtain cynandione A. The preparation method of cynandione A has the advantages of high efficiency, short period, low pollution and simple processes, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of natural medicine chemistry, and in particular relates to a preparation method of radix diketone A. Background technique [0002] Baishouwu diketone A (cynandione A) is a kind of acetophenone compound prepared from Baishouwu, CAS No. 168706-29-4, molecular formula C16H14O6, molecular weight 302.28, molecular structure: [0003] [0004] Baishouwu is the root tuber of the Radixaceae plant Niupixiao and Jiye Niupixiao, also known as Geshanxiao ("Compendium"), Baihewu, Baiheshouwu ("Eastern Medicine Shoushiyuan"), Geshanzhe ("Classification of Herbal Medicines") "), Baimuxiang, Wild Sweet Potato (Zhejiang), Yizhong Sanxiao (Hunan), Peace Ginseng, Sanhuaqi (Guangdong), Zhang Guolao (Jiangxi), have the functions of nourishing liver and kidney, benefiting essence and blood, strengthening muscles and bones, and stopping pain. heartache. It is often used for dizziness, insomnia, forgetfulness, premature graying of bear...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/83C07C45/79C07C45/78
CPCY02P20/141Y02P20/54
Inventor 陈洪生程志鹏
Owner 江苏博益生物科技有限公司
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