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Method for extraction and separation of chlorogenic acid, pinoresinol diglucoside, aucubin and gutta-percha from eucommia ulmodies oliv raw material

A technology of pinoresinol diglucoside and aucubin, applied in chemical instruments and methods, separation/purification of carboxylic acid esters, sugar derivatives, etc., can solve the problems of cumbersome operation, high cost, waste of active ingredients, etc. Achieve simple operation, low cost, and meet the effect of industrial large-scale application

Active Publication Date: 2015-04-08
MICOLTA BIORESOURCE INC LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the existing technology for the separation of active ingredients in Eucommia, there are a series of defects such as the inability to obtain multiple types of active ingredients at the same time, resulting in waste of active ingredients, complicated process, cumbersome operation, low yield of active ingredients of the drug obtained, and high cost. The purpose of the present invention is to provide a method for extracting and separating high-purity chlorogenic acid, pinoresinol diglucoside, aucubin and eucommia gum from Eucommia ulmoides at a higher yield. The method is simple to operate and low in cost. Comprehensive utilization of natural resources to meet the needs of industrialized production

Method used

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  • Method for extraction and separation of chlorogenic acid, pinoresinol diglucoside, aucubin and gutta-percha from eucommia ulmodies oliv raw material
  • Method for extraction and separation of chlorogenic acid, pinoresinol diglucoside, aucubin and gutta-percha from eucommia ulmodies oliv raw material
  • Method for extraction and separation of chlorogenic acid, pinoresinol diglucoside, aucubin and gutta-percha from eucommia ulmodies oliv raw material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Extraction: Weigh 50kg of fresh bark of Eucommia ulmoides, cut it into 5-10cm sections with a medicine cutter, then pulverize it into a coarse powder through a hammer mill, put it into a multi-functional extraction tank, add 80% methanol and stir and reflux for extraction twice, Add 200L for the first time, extract for 2 hours, add 150L for the second time, extract for 1 hour, the extract is discharged through the screen at the bottom of the tank, filtered through a pipeline filter, and the extracts are collected twice and combined. After methanol is recovered from the extraction residue, it is used for later use. Concentrate the extract under reduced pressure to 25L, transfer it to an alcohol sink, add 25L of water, heat to 80°C, stir for 30min, cool to 8-10°C, let stand for 12h, and then centrifuge through a three-legged centrifuge bag to obtain centrifuged liquid.

[0033] Enrichment: The centrifugate is completely absorbed by D101 macroporous resin, washed with wat...

Embodiment 2

[0037]Extraction: Weigh 200kg of Eucommia ulmoides bark commercially available, cut into 5-10cm sections with a medicine cutter, then pulverize into coarse powder with a hammer mill, put it into a multi-functional extraction tank, add 70% ethanol to stir and reflux for extraction twice , add 1600L for the first time, extract for 2 hours, add 1200L for the second time, extract for 1 hour, the extract is discharged through the screen at the bottom of the tank, filtered through a pipeline filter, and the two extracts are collected and combined. Extract the residue to recycle ethanol and keep it for later use. Concentrate the extract to 200L under reduced pressure, transfer it to an alcohol precipitation tank, add 200L water, heat to 85°C, stir for 30min, cool to 10-15°C, let stand for 24h, and then centrifuge through a three-legged centrifuge bag to obtain centrifuged liquid.

[0038] Enrichment: Adsorb the centrifugate completely through alumina, wash with water until colorless...

Embodiment 3

[0043] Extraction: Weigh 20kg fresh and dried skin of Eucommia ulmoides, slice it, stir fry it in a frying pan for 30 minutes, and then pulverize it into a coarse powder through a hammer mill, put it into a multi-functional extraction tank, add acetone to stir and reflux for extraction twice, the first Add 80L for the first time, extract for 2 hours, add 60L for the second time, extract for 1 hour, the extract is discharged through the screen at the bottom of the tank, filtered through a pipeline filter, and the extracts are collected twice and combined. The acetone is recovered from the extraction residue, which is set aside. Concentrate the extract to 10L under reduced pressure, transfer it to an alcohol sink, add 10L of water, heat to 80°C, stir for 30min, cool to 8-10°C, let stand for 12h, and then centrifuge through a three-legged centrifuge bag to obtain centrifuged liquid.

[0044] Enrichment: The centrifugate is completely absorbed by D101 macroporous resin, washed wi...

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Abstract

The invention discloses a method for extraction and separation of chlorogenic acid, pinoresinol diglucoside, aucubin and gutta-percha from a eucommia ulmodies oliv raw material. The method comprises the steps: extracting from the eucommia ulmodies oliv raw material by an organic solvent, concentrating, successively carrying out hot water dissolving, cold precipitation and centrifugal separation on the concentrate to obtain a centrifugal liquid, carrying out enrichment, elution and concentration on the centrifugal liquid, to obtain an eucommia ulmodies oliv extract, separating and purifying the eucommia ulmodies oliv extract, and thus respectively obtaining the pinoresinol diglucoside, chlorogenic acid and aucubin; and carrying out hydrolysis and organic solvent extraction on the extract residue, to obtain the gutta-percha. The method extracts and separates the high-purity chlorogenic acid, pinoresinol diglucoside, aucubin and gutta-percha from the eucommia ulmodies oliv with relatively high yield simultaneously, has the advantages of simple operation and low cost, realizes the comprehensive utilization of natural resources, and meets industrialized production.

Description

technical field [0001] The invention relates to a method for simultaneously separating and purifying chlorogenic acid, pinoresinol diglucoside, aucubin and eucommia gum from Eucommia ulmodies Oliv., belonging to the field of natural medicine extraction. Background technique [0002] Eucommia ulmoides is a plant of the genus Eucommia in the family Eucommia. It is a perennial deciduous tree unique to my country. It is distributed in Shaanxi, Gansu, Henan, Hubei, Sichuan, Yunnan, Guizhou, Hunan and Zhejiang provinces, and is now widely planted in various places. In the natural state, it grows in low mountains, valleys or low-slope forests at an altitude of 300-500 meters. The selection of soil is not strict, and it can grow on barren red soil or rocky cliffs. The bark is used medicinally, as a tonic and lowers blood pressure, and can treat low back pain, rheumatism and habitual abortion. The chemical composition of Eucommia ulmoides is very complex. The chlorogenic acid in the...

Claims

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Application Information

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IPC IPC(8): C07C69/732C07C67/48C07H15/26C07H17/04C07H1/08C08J3/00C08L7/00
CPCC07C67/48C07H1/08C07H15/26C07H17/04C08J3/00C08J2307/00C07C69/732
Inventor 欧阳勇曾建国
Owner MICOLTA BIORESOURCE INC LTD
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