Crotepoxide preparation method

A technology for the preparation of echinoulenin, stems and leaves, which can solve the problems of complex purification process, serious pollution, and low energy efficiency of the extraction method, and achieve high extraction efficiency and simple process operation , The effect of high product yield

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

AI Technical Summary

Problems solved by technology

[0005] Existing methods for the preparation of fennelidin mostly use conventional reagents for extraction, the extraction method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Take 3 kg of sea wind rattan stems and leaves and grind them into 60 meshes, put them into a supercritical CO2 extraction kettle, feed liquid CO2, set the pressure at 25 MPa, temperature at 45 ° C, and flow rate at 4 ml / g / min, after dynamic equilibrium, feed ethyl acetate solution , the flow rate is 0.2ml / g / min, extract for 60min, and analyze under the conditions of pressure 5MPa and temperature 60℃, the obtained extract is dissolved in 70% ethanol solution, refluxed with 2% activated carbon for decolorization, the decolorized solution is concentrated and then extracted with ethyl acetate , place the extract to 1 / 4 volume to crystallize, then dissolve the crystals with 90% ethanol, pass through a short column of neutral alumina resin (120 mesh), collect the next column liquid, concentrate the crystals, and dry to obtain 1.1 g, content 97.2%.

Embodiment 2

[0018] Take 3 kg of sea wind rattan stems and leaves and grind them into 80 meshes, put them into a supercritical CO2 extraction kettle, feed liquid CO2, set the pressure at 20 MPa, temperature at 55 ° C, and flow rate at 2 ml / g / min, after dynamic equilibrium, feed ethyl acetate solution , the flow rate is 0.3ml / g / min, extract for 40min, and analyze under the conditions of pressure 6MPa and temperature 50℃, the obtained extract is dissolved in 80% ethanol solution, added with 3% activated carbon to reflux for decolorization, and the decolorized solution is concentrated and then extracted with ethyl acetate , put the extract to 1 / 3 volume to crystallize, and then dissolve the crystals with 95% ethanol, pass through a short column of neutral alumina resin (180 mesh), collect the next column liquid, concentrate the crystals, and dry to obtain 1.3 g, content 98.3%.

Embodiment 3

[0020] Take 3 kg of sea wind rattan stems and leaves and grind them into 20 meshes, put them into a supercritical CO2 extraction kettle, feed liquid CO2, set the pressure at 30 MPa, temperature at 40 ° C, and flow rate at 5 ml / g / min, after dynamic equilibrium, feed ethyl acetate solution , the flow rate is 0.2ml / g / min, extract for 50min, and analyze under the conditions of pressure 5MPa and temperature 50℃, the obtained extract is dissolved in 80% ethanol solution, refluxed with 1% activated carbon for decolorization, the decolorized solution is concentrated and then extracted with ethyl acetate , put the extract to 1 / 6 volume for crystallization, dissolve the crystallization with 95% ethanol, pass through a short column of neutral alumina resin (100 mesh), collect the next column liquid, concentrate the crystallization, and dry to obtain 1g of betelene , content 97.1%.

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Abstract

The present invention discloses a crotepoxide preparation method, which comprises: A, taking stems and leaves of Caulis Piperis Kadsurae, crushing to achieve 20-80 mesh, pouring into a supercritical CO2 extraction kettle, introducing liquid-state CO2 and an entrainer, extracting for 30-60 min at a temperature of 40-55 DEG C under a pressure of 20-30 MPa, and resolving at a temperature of 40-60 DEG C under a pressure of 5-9 MPa to obtain an extract; and B, dissolving the extract with an ethanol solution, adding active carbon, carrying out reflux decolorizing, concentrating the decolorizing solution, extracting with ethyl acetate, carrying out concentration crystallization on the extraction solution, dissolving the crystal with ethanol, loading onto an alumina resin short column, collecting the lower column liquid, and carrying out concentration crystallization and drying to obtain the finished product. The crotepoxide preparation method of the present invention has characteristics of high extraction efficiency, simple preparation process, and easy industrial production achieving.

Description

technical field [0001] The invention belongs to the field of biotechnology, and in particular relates to a preparation method of betelene. Background technique [0002] Pinotiflorin, molecular formula C18H18O8, molecular weight 362.33, CAS number 20421-13-0, molecular structural formula [0003] [0004] Seawind Teng is a plant of the family Piperaceae. Its stems and leaves contain Echinoside, Echinotenone, Echinoquinone, and Echinoside amide. Betone has the highest content and has the effect of suppressing tumors. [0005] Existing methods for the preparation of betelene generally use conventional reagents for extraction. The extraction method has low energy efficiency, serious pollution, and complicated purification process, and no industrialized method has been disclosed. Contents of the invention [0006] The purpose of the present invention is to overcome the defects and deficiencies of the prior art, and provide a method for industrialized preparation of bet...

Claims

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Application Information

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IPC IPC(8): C07D493/04
CPCC07D493/04Y02P20/54
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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