Method for separating and purifying chlorogenic acid from eucommia ulmoides leaves

A technology of chlorogenic acid and eucommia leaves, which is applied in the field of steam explosion-assisted extraction of chlorogenic acid in eucommia leaves and separation and purification of chlorogenic acid, which can solve the problems of unstable structure of catechol, easy oxidation and decomposition, etc., and achieve treatment The effect of short time, improving extraction rate and avoiding loss

Inactive Publication Date: 2012-02-15
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Chlorogenic acid is easily soluble in hot water, but due to the unstable structure of catechol in chlorogenic acid, it is easy to oxidize and decompose under high temperature and long-term heating. T...

Method used

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  • Method for separating and purifying chlorogenic acid from eucommia ulmoides leaves
  • Method for separating and purifying chlorogenic acid from eucommia ulmoides leaves
  • Method for separating and purifying chlorogenic acid from eucommia ulmoides leaves

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Take 500g of Eucommia ulmoides leaf medicinal materials, add eucommia ulmoides leaf medicinal materials to acidic water (pH adjusted to 3.5 by acetic acid) in a ratio of 1:1 by mass of absolute dry medicinal materials to acidic water, and then soak for 30min at room temperature; place the soaked materials In the steam explosion tank, first pass air and then liquid nitrogen to make the temperature in the tank reach 100°C, maintain it for 3 minutes, and then perform steam explosion treatment; add the steam explosion treatment material or the conventionally crushed material to 40 mesh into it. 3 times the weight of water, extract 3 times at 60°C, 60 min each time, combine the extracts; concentrate the extracts under reduced pressure, add 3 times the concentrated liquid ethyl acetate and extract twice to obtain the ethyl acetate layer, to which 5 %NaOH liquid neutralization makes the chlorogenic acid in ethyl acetate enter the water phase. After the water phase is separated, ...

Embodiment 2

[0030] Take 500g of Eucommia ulmoides leaf medicinal material, add eucommia ulmoides leaf medicinal material to acidic water (pH is adjusted to 3.0 by hydrochloric acid) in a ratio of 1:2 by mass of absolute dry medicinal material and acidic water, and then soak for 60min at room temperature; place the soaked material Put carbon dioxide into the steam explosion tank, make the temperature in the tank reach 80℃, maintain it for 15 minutes, then proceed with steam explosion treatment; add the material after steam explosion treatment or the conventionally crushed material to 40 mesh into water 5 times its absolute dry weight. Extract 3 times at 40°C for 50 minutes each time, combine the extracts; concentrate the extracts under reduced pressure, add 3 times the concentrated solution of ethyl acetate and extract twice to obtain the ethyl acetate layer, which is added with 3% NaOH solution to neutralize the acetic acid The chlorogenic acid in the ethyl ester enters the water phase. Aft...

Embodiment 3

[0032] Take 500g of Eucommia ulmoides leaf medicinal material, add eucommia ulmoides leaf medicinal material to acidic water (pH 2.0 adjusted by sulfuric acid) in a ratio of 1:3 by mass of absolutely dry medicinal material and acidic water, and then soak for 5min at room temperature; place the soaked material in In the steam explosion tank, pass nitrogen first, then liquid nitrogen, so that the temperature in the tank reaches 75℃, maintain it for 10 minutes, and then perform steam explosion treatment; add the material after steam explosion treatment or the conventionally crushed material to 40 mesh into its absolute dryness 10 times the weight of water was extracted 3 times at 80°C for 30 minutes each time, and the extracts were combined; the extracts were concentrated under reduced pressure, and 3.5 times the ethyl acetate of the concentrated solution was added for extraction twice to obtain an ethyl acetate layer. %NaOH liquid neutralization makes the chlorogenic acid in ethyl...

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Abstract

Based on the instable structure of o-dihydroxybenzene in chlorogenic acid and easily decomposed and oxidizable characteristics if chlorogenic acid is heated at high temperature for a long time, the invention discloses a steam explosion assisted method for extracting and purifying chlorogenic acid from eucommia ulmoides leaves, comprising the following steps of: placing the eucommia ulmoides leaves, which have been pre-immersed in acid water at the pH of 2.0-6.5 for 5-180 min, into a steam explosion tank; allowing one or any two combined steam explosion mediums selected from air, carbon dioxide, ozone, liquid nitrogen, nitrogen, steam, supercritical CO2 and ethanol to enter; carrying out steam explosion treatment at the temperature of 30-100 DEG C for 1-30 min; adding the material which has undergone the steam explosion treatment into hot water, directly extracting chlorogenic acid, merging extracts and purifying to obtain the chlorogenic acid quality goods. By multimedium combined low temperature steam explosion pretreatment, the stability of the active component chlorogenic acid is protected, and simultaneously the cell wall of the eucommia ulmoides leaves is effectively destroyed, so as to primarily release the influence of the compact cell-wall structure of the eucommia ulmoides leaves on the dissolution of chlorogenic acid during extraction and raise the recovery rate of chlorogenic acid in the eucommia ulmoides leaves. The invention provides a new technological approach for high-efficiency comprehensive utilization of eucommia ulmoides leaves.

Description

Technical field [0001] The invention belongs to the technical field of Chinese herbal medicine processing, and particularly relates to a method for steam explosion to assist in extracting chlorogenic acid from Eucommia ulmoides leaves and separating and purifying the chlorogenic acid. Background technique [0002] Chlorogenic acid is a substance with a wide range of physiological and pharmacological activities. It has the effects of choleretic, antibacterial, hypotensive, white blood cell increase and central nervous stimulation. It is one of the effective ingredients of many Chinese herbal medicines, and it is also a certain patent medicine. Quality indicators. Chlorogenic acid is widely used in medicine, daily chemical and food industries. [0003] The extraction of plant active ingredients such as chlorogenic acid is a process that breaks through the dense barrier of cell walls and effectively dissolves, increasing the degree of fragmentation of plant cells, which will directly...

Claims

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Application Information

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IPC IPC(8): C07C69/732C07C67/52
CPCY02P20/54
Inventor 陈洪章付小果
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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