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Cucurbitacins preparation method

A technology of snow cholestyramine and snow cholestasis, which is applied in the field of preparation of leucobilin A, and achieves the effects of short cycle, high efficiency and easy purification.

Inactive Publication Date: 2015-09-16
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

No disclosure of a process for the preparation of pectin A was found

Method used

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  • Cucurbitacins preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0013] Get 2kg snow gall raw material and pulverize 60 meshes, put into supercritical CO2 extraction kettle, pass into liquid CO2, flow rate is 2ml / min / g raw material, pass into methanol as entrainer, flow rate is 0.3ml / min / g, at pressure 21MPa, Under the condition of temperature of 50°C, extract for 100 minutes, analyze the extract, heat dissolve with 90% ethanol and add an equal volume of petroleum ether, then add 1 / 3 volume of aqueous solution, mix well, static layer, collect the petroleum ether layer to recover the reagent, Reflux and dissolve with 90% ethanol solution, then add activated carbon to decolorize, concentrate 1 / 4 volume of the decolorization solution and place it to crystallize, then recrystallize the crystals with 95% ethanol solution, and dry to obtain 6 g of ichorin A, which is detected by high performance liquid phase. 98.3%.

Embodiment 2

[0015] Get 2kg snow gall raw material and pulverize 60 meshes, put into supercritical CO2 extraction kettle, pass into liquid CO2, flow rate is 1ml / min / g raw material, pass into methanol as entrainer, flow rate is 0.2ml / min / g, at pressure 25MPa, Under the condition of 45°C, extract for 60 minutes, analyze the extract, heat dissolve it with 95% ethanol and add an equal volume of petroleum ether, then add 1 times the volume of aqueous solution, mix well, static layer, collect the petroleum ether layer to recover the reagent, and then Reflux and dissolve with 95% ethanol solution, add activated carbon to reflux for decolorization, concentrate 1 / 4 volume of the decolorization solution and place it for crystallization, then recrystallize the crystals with 90% ethanol solution, dry to obtain 5.6 g of ichorin A, which is detected by high performance liquid phase. The content is 97.3%.

Embodiment 3

[0017] Get 2kg snow gall raw material and pulverize 40 meshes, put into supercritical CO2 extraction kettle, pass into liquid CO2, flow rate is 5ml / min / g raw material, pass into methanol as entrainer, flow rate is 0.1ml / min / g, at pressure 15MPa, Under the condition of temperature 30°C, extract for 150min, analyze the extract, heat dissolve with 95% ethanol and add an equal volume of petroleum ether, then add 1 / 2 volume of aqueous solution, mix well, static layer, collect the petroleum ether layer to recover the reagent, Reflux and dissolve with 95% ethanol solution, add activated carbon to reflux for decolorization, concentrate 1 / 3 of the volume of the decolorization solution and place it for crystallization, then recrystallize the crystals with 95% ethanol solution, dry to obtain 6.7g of ichorin A, which is detected by high performance liquid phase , content 97.5%.

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Abstract

The present invention discloses a cucurbitacins preparation method, which comprises: 1) taking a Hemsleya chinensis raw material, crushing, adding to a supercritical CO2 extraction kettle, setting the temperature of 30-50 DEG C and the pressure of 15-25 MPa, introducing liquid-state CO2, concurrently introducing methanol as an entrainer, extracting for 30-150 min, and resolving to obtain an extract, wherein the liquid-state CO2 flow rate is 1-5 ml / min / g of raw material, and the methanol flow rate is 0.1-0.3 ml / min / g; and 2) carrying out hot dissolving on the extract with ethanol, adding an equal volume of petroleum ether, adding a proper amount of an aqueous solution, collecting the petroleum ether layer to recover the reagent, adding an ethanol solution to carry out reflux dissolving, adding active carbon to decolorize, carrying out concentration crystallization on the decolorizing solution, re-crystallizing with an ethanol solution, and drying to obtain the finished product. The cucurbitacins preparation method of the present invention has characteristics of high extraction efficiency, simple purification process, and environmental protection, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of biological technology, and in particular relates to a preparation method of pectin A. Background technique [0002] Cucurbitacins, English name Cucurbitacins, molecular formula C30H42O6, molecular weight 498.656, CAS number 60137-06-6, molecular structural formula: [0003] [0004] Snow gallbladder is a plant of the genus Snow gallbladder in Cucurbitaceae, which has the effects of reducing heat and detoxification, antibacterial and anti-inflammatory. For the treatment of bacillary dysentery, enteritis, bronchitis, acute tonsillitis. Snow gall tubers contain snow gallin A, snow gallin B, bamboo ginsenoside, oleanolic acid-β-glucose ester, etc. Among them, gentianin is the main functional component, which is a mixture of gentianin A and gentianin B extracted from plants of the genus genus cucurbitaceae. Snow gallin A has heat-clearing and detoxifying, antibacterial and anti-inflammatory functions. Existing te...

Claims

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Application Information

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IPC IPC(8): C07J71/00C07J9/00
CPCC07J9/00C07J71/0005Y02P20/54
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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