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Method for preparing arctigenin from burdock

A technology for arctigenin and arctium seed, which is applied in the field of preparation of arctigenin in a process, can solve the problems of low extraction rate, unsatisfactory enzymatic hydrolysis conditions and purification process, and achieves reduction of enzyme dosage, improvement of enzymatic hydrolysis efficiency and product content. Effect

Inactive Publication Date: 2010-06-23
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

There is also supercritical fluid extraction, the extraction rate is low
Both Xu Feiyi et al.’s publications “Research on Microbial Fermentation Transformation of Arctium Fructus” and Bai Jiafeng’s “Research on Microbial Fermentation Transformation of Arctium Fructus” disclose enzyme fermentation transformation, but the enzymatic hydrolysis conditions and purification process are not ideal

Method used

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  • Method for preparing arctigenin from burdock
  • Method for preparing arctigenin from burdock

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Take burdock fruit, crush it to 30 mesh, take 10kg, add 80L80% methanol for reflux extraction for 2 hours, extract twice, combine to obtain 140L extract, add 800g activated carbon for decolorization for 1 hour, filter the decolorized solution through a microfiltration membrane, and then filter the filtrate again Through a hollow ultrafiltration membrane with a molecular weight cut-off of 6000-10000, ultrafiltration at a pressure of 0.8Mpa, the permeate is concentrated to no alcohol, the concentrated solution emits hydrochloric acid to adjust the pH to 5, add 20g of compound enzyme, keep warm at 50°C, and then use 30 Rotate per minute and stir the enzymolysis for 24 hours, centrifuge the enzymolysis solution, dissolve the centrifuge with chloroform reflux, filter, and place to crystallize to obtain 423g of arctigenin crude crystals, with a content of 73%; the crude crystals are sequentially used with 90% and 99% % Methanol was refluxed to dissolve, left to stand for cryst...

Embodiment 2

[0040] Take burdock fruit, crush it to 40 mesh, take 10kg, add 60L of 75% methanol to reflux for extraction for 1 hour, extract 3 times, combine to obtain 160L extract, add 900g of activated carbon for decolorization for 1.5 hours, filter the decolorized solution through a microfiltration membrane, collect the transparent After passing through the liquid, the filtrate passes through a hollow ultrafiltration membrane with a molecular weight cut-off, ultrafiltration at a pressure of 0.4Mpa, concentrates the permeated liquid to no alcohol, collects the concentrated liquid, adjusts the pH to 5.5 with hydrochloric acid, adds 12g of compound enzyme, and incubates at 55°C , stir the enzymolysis with 20 rpm for 26 hours, centrifuge the enzymolysis solution, dissolve the centrifuge with chloroform reflux, filter and place it to crystallize, and get 413g of arctigenin crude crystals, with a content of 71%; the crude crystals are successively washed with 90% Reflux with 99% methanol to di...

Embodiment 3

[0042] Take burdock fruit, crush it to 10 mesh, take 10kg, add 70L of 80% methanol for reflux extraction for 1 hour, extract 3 times, combine to obtain 190L extract, add 1000g of activated carbon for decolorization for 2 hours, filter the decolorized solution through a microfiltration membrane, and then filter the filtrate again Through the ultrafiltration membrane, ultrafiltration at a pressure of 0.6Mpa, concentrate the permeate to no alcohol, collect the concentrated solution, adjust the pH to 6 with hydrochloric acid, add 20g of compound enzyme, keep warm at 45°C, and stir at 25 rpm for enzymolysis For 20 hours, centrifuge the enzymolyzate, dissolve the centrifugate with chloroform, and place to crystallize to obtain 418g of arctigenin crude crystals, with a content of 72%. The crystals were obtained and dried to obtain 240 g of arctigenin with a content of 98.9%.

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Abstract

The invention relates to a method for preparing arctigenin from burdock. A process of the method comprises: taking burdock medicinal materials as raw materials; grinding the raw materials; performing methanol reflux extraction for 2 to 3 times; performing activated carbon decolorizing; concentrating the obtained product to have no alcohol after microfiltration and ultrafiltration; regulating pH; adding compound enzyme and stirring for enzymatic hydrolysis; centrifuging the obtained product; dissolving centrifugation objects in chloroform; standing the obtained product for crystallization; and dissolving coarse crystals in 90 percent methanol and 99 percent methanol for recrystallization. The process has the advantages of simple operation and short cycle.

Description

Technical field: [0001] The invention relates to a method for preparing arctigenin from burdock seeds, in particular to a method for preparing arctigenin by membrane separation, compound enzymatic hydrolysis and the like. Background technique: [0002] arctigenin [0003] chemical name: [0004] (3R,4R)-4-[(3,4-Dimethoxyphenyl)methyl]dihydro-3-[(4-hydroxy-3-methoxyphenyl)methyl]-2(3H)-furanone [0005] Molecular formula: C 21 h 24 o 6 [0006] Molecular weight: 372.41 [0007] Molecular Structure: [0008] [0009] Physical properties: colorless, odorless crystal; insoluble in water, easily soluble in methanol, chloroform and other organic solvents. [0010] Arctigenin has strong pharmacological activities in anti-inflammatory, anti-virus, anti-tumor, immune regulation, etc.; at the same time, it can be used as a new type of heat shock response inhibition regulator, which is effective in the treatment of cancers manifested by hyperthermia. help. In addition, it ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C12P17/04C07D307/33
Inventor 刘东锋张翼杨成东
Owner NANJING ZELANG MEDICAL TECH
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