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Preparation method of arctigenin

A technology of arctigenin and arctium seed is applied in the field of preparation of arctigenin, can solve the problems of unsafe, unfavorable industrialized production, high price and the like, and achieves the effect suitable for industrialized production

Inactive Publication Date: 2010-06-16
LIAONING UNIV OF TRADITIONAL CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The previous process generally required degreasing before extracting arctiin, and the solvent used for degreasing was a flammable and explosive organic solvent, which was not only expensive, but also unsafe, which was not conducive to industrial production

Method used

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  • Preparation method of arctigenin
  • Preparation method of arctigenin

Examples

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Effect test

Embodiment 1

[0016] Take 100 grams of burdock fruit, crush it, pass it through a 10-mesh sieve, add 500 ml of water, enzymolyze it at 25°C for 2 hours, let it rest, and filter. Concentrate the filtrate to about one-third under reduced pressure, add ethanol to make a 20% ethanol aqueous solution, add it to the medicinal material residue, reflux for extraction for 1 hour, and filter. The residue was further extracted with 20% ethanol twice for one hour each time. The combined extracts were concentrated to near dryness under reduced pressure. Then column chromatography separation was performed 3 times. Mix the sample with the same amount of sample mixing silica gel (100-120 mesh) as the extract each time, and the column chromatography silica gel is 10 times the sample amount. Elute with chloroform-methanol, the volume ratio of chloroform-methanol is 100:0-95:5. Fractions containing arctigenin were combined and evaporated to dryness. Repeated recrystallization with methanol or ethanol (95%...

Embodiment 2

[0018] Take 100 grams of burdock fruit, crush it, pass it through a 60-mesh sieve, add 1500 ml of water, enzymolyze it at 35°C for 12 hours, let it rest, and filter. Concentrate the filtrate to about one-third under reduced pressure, add ethanol to form a 60% ethanol aqueous solution, add it to the medicinal material residue, reflux for extraction for 3 hours, and filter. The residue was further extracted with 30% ethanol twice for one hour each time. The combined extracts were concentrated to near dryness under reduced pressure. Then column chromatography separation was performed twice. Mix the sample with the same amount of sample mixing silica gel (100-120 mesh) as the extract each time, and the column chromatography silica gel is 5 times the sample amount. Elute with chloroform-methanol, the volume ratio of chloroform-methanol is 100:0-95:5. Fractions containing arctigenin were combined and evaporated to dryness. Repeated recrystallization with methanol or ethanol (95%...

Embodiment 3

[0020] Take 100 grams of burdock fruit, crush it, pass it through a 20-mesh sieve, add 1000 ml of water, enzymolyze it at 50°C for 8 hours, let it rest, and filter. The filtrate was concentrated under reduced pressure to nearly dryness, added 95% ethanol aqueous solution, added to the medicinal material residue, extracted under reflux for 3 hours, and filtered. The residue was extracted twice with 95% ethanol for one hour each time. The combined extracts were concentrated to near dryness under reduced pressure. Then column chromatography separation was performed twice. Mix the sample with the same amount of sample mixing silica gel (100-120 mesh) as the extract each time, and the column chromatography silica gel is 20 times the sample amount. Elute with chloroform-methanol, the volume ratio of chloroform-methanol is 100:0-95:5. Fractions containing arctigenin were combined and evaporated to dryness. Repeated recrystallization with methanol or ethanol (95%, analytically pur...

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Abstract

The invention relates to a preparation method of arctigenin, which comprises the following steps: after pulverizing great burdock fruit, carrying out zymohydrolysis according to a self inherent hydrolase; extracting the medicinal material after zymohydrolysis to obtain a crude extract of the arctigenin and then purifying the crude extract of the arctigenin by a silica gel column chromatography method and a solvent recrystallization method to obtain a purified product of the arctigenin. The purity of the arctigenin is greater than or equal to 98%, and the yield is more than 2%. The arctigenin can be used as a bulk drug and is applied to the medicaments of various relevant diseases. The preparation method of the arctigenin has the advancement and the practical value that the method does not need to adopt an inflammable and explosive organic solvent to degrease the medicinal material, and the self inherent hydrolase of the great burdock fruit is also utilized to directly prepare the arctigenin from the medicinal material. The method is simple, convenient and practical and is more suitable for industrialized production. The preparation method adopts the self inherent hydrolase of the medicinal material for preparation and converts a compound, which is very rare at home and abroad at present.

Description

technical field [0001] The invention relates to a preparation method of a drug raw material, in particular to a new preparation method of arctigenin (English name, Arctigenin). The method of the invention refers to the method of hydrolyzing the arctiin in the medicinal material into arctigenin by the hydrolase existing in the arctium fruit itself, and then combining the chromatographic separation method to directly produce the arctigenin from the arctium fruit medicinal material. [0002] The advancement and practical value of the method for preparing arctigenin of the present invention are that the method does not need to use flammable and explosive organic solvents to degrease the medicinal materials, and at the same time, the inherent hydrolytic enzyme of arctium itself is used to directly prepare burdock from medicinal materials. Aglycone. The method is simple and practical, and is more suitable for industrial production. At present, it is rare to use the hydrolytic enzy...

Claims

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Application Information

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IPC IPC(8): C12P17/04A61K31/365A61P35/00A61P31/00A61P29/00A61P31/12
CPCY02P20/54
Inventor 窦德强侯蔷康廷国李鸿福
Owner LIAONING UNIV OF TRADITIONAL CHINESE MEDICINE
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