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Preparation method of corilagin

A supercritical, pore adsorption technology, applied in the preparation of sugar derivatives, chemical instruments and methods, production of bulk chemicals, etc., can solve problems such as the lack of reports on large-scale industrial production and preparation of high-purity corylazine, and achieve the benefits of large-scale production. Production operation, less pollution and less energy consumption

Inactive Publication Date: 2011-04-20
SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the prior art, there is no report on the preparation process applicable to the large-scale industrial production of high-purity Corilagin

Method used

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  • Preparation method of corilagin

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Effect test

Embodiment 1

[0026] Get phylloxera coarse powder 10Kg, join in CO 2 In the supercritical extractor, ethyl acetate is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 3%, the extraction pressure is 10MPa, the temperature is 35°C, and the CO 2 Flow rate 1ml / g crude drug min, extraction time 80min, get extract, add water to dissolve, filter, filtrate is adsorbed by HPD700 type macroporous adsorption resin, 20% ethanol is eluted, collects the eluent of 3 times of column volume, reduces Recover ethanol under pressure and concentrate, add acetic acid to the concentrated solution to adjust the pH to 4-4.5, carry out 6-stage countercurrent extraction with ethyl acetate-water mixed solvent with a ratio of 10:2, the volume ratio of the concentrated solution to the total amount of mixed solvent is 1: 6. Combine the extracts, recover the solvent under reduced pressure, add absolute ethanol to crystallize, separate the crystals, wash, and dry to obtain...

Embodiment 2

[0028] Get phylloxera coarse powder 10Kg, join in CO 2 In the supercritical extractor, ethyl acetate is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 8%, the extraction pressure is 30MPa, the temperature is 55°C, and the CO 2 Flow rate 3ml / g crude drug min, extraction time 150min, get extract, add water to dissolve, filter, filtrate is adsorbed by H50 type macroporous adsorption resin, eluted with 60% ethanol, collects the eluate of 8 times of column volume, reduces Recover ethanol under pressure and concentrate, add acetic acid to the concentrated solution to adjust the pH to 4-4.5, carry out 10-stage countercurrent extraction with ethyl acetate-water mixed solvent with a ratio of 10:2, the volume ratio of the concentrated solution to the total amount of mixed solvent is 1: 10. Combine the extracts, recover the solvent under reduced pressure, add absolute ethanol to crystallize, separate the crystals, wash, and dry to obta...

Embodiment 3

[0030] Get phylloxera coarse powder 10Kg, join in CO 2 In the supercritical extractor, ethyl acetate is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 5%, the extraction pressure is 20MPa, the temperature is 45°C, and the CO 2 Flow rate 2ml / g crude drug min, extraction time 100min, get extract, add water to dissolve, filter, filtrate is absorbed by AB8 type macroporous adsorption resin, 40% ethanol elutes, collects the eluent of 5 times of column volume, reduces Recover ethanol under pressure and concentrate, add acetic acid to the concentrated solution to adjust the pH to 4-4.5, carry out 8-stage countercurrent extraction with ethyl acetate-water mixed solvent with a ratio of 10:2, the volume ratio of the concentrated solution to the total amount of mixed solvent is 1: 8. Combine the extracts, recover the solvent under reduced pressure, add absolute ethanol to crystallize, separate the crystals, wash, and dry to obtain 12.4...

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Abstract

The invention relates to a preparation method of corilagin, wherein the preparation method is simple and convenient in operation, less in pollution and low in energy consumption. The preparation method comprises the following process steps: taking coarse powder of phyllanthus urinaria; adding the coarse powder of phyllanthus urinaria into a CO2 supercritical extractor for extracting to obtain an extract; adding water for dissolving; filtering; adsorbing the filtered solution by macroporous absorption resin; eluting by ethanol; collecting the eluent; recovering the ethanol at the reduced pressure, and concentrating the ethanol; adding acetic acid into the concentrated solution for regulating the pH to 4-4.5; carrying out 6-10-grade counter-current extraction by a mixed solvent formed by mixing ethyl acetate and water based on the ratio of 10:2, wherein the volume ratio of the concentrated solution to the total dosage of the mixed solvent is (1:6)-10; mixing the extracted solutions; recovering the solvent at the reduced pressure; adding absolute ethanol for crystallizing; and separating the crystal, washing and drying to obtain a finished product. By using the method provided by the invention for preparing the corilagin, the product purity is high, and the industrialized amplification can be realized easily.

Description

technical field [0001] The invention relates to a preparation method of corilagin, in particular to a preparation method of extracting corilagin from plants. Background technique [0002] Corilagin (Corilagin), alias: tanned porphyrin, tanned material pruritin, molecular formula: C 27 h 22 o 18 , Molecular weight: 634.46, CAS accession number: 23094-69-1, present in various plants of the family Genusiaceae, thistle family, and pomegranate family. Among them, Phyllanthus urinaria L. is rich in the plant Phyllanthus urinaria L. Its molecular formula is as follows: [0003] [0004] Modern studies have shown that corilagin has strong antiviral, antibacterial, anti-inflammatory, and hepatitis treatment activities, and it is also used as a raw material for the synthesis of other active derivatives. [0005] Phyllanthus urinaria L., a traditional Chinese medicine, is the whole herb of Phyllanthus urinaria L., a plant in the family of thistle family. [0006] In the prior ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H13/08C07H1/08
CPCY02P20/54
Inventor 王峰王琳张发成
Owner SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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