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Method for non column chromatography separation and purification of witloof acid from Echinacea purpurea extractive

A technology of echinacea purpurea extract and chromatographic separation, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of cumbersome column chromatography operation steps, high requirements for chromatographic equipment, difficult industrial production, etc., and achieve easy continuous The effect of efficient operation, cost reduction and high recovery rate

Inactive Publication Date: 2011-08-24
HUNAN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the requirements for chromatographic equipment are high, the cost is high, and it is not easy to scale up. In particular, the operation steps of column chromatography are cumbersome, time-consuming and laborious, and the recovery rate is low, so it is difficult to achieve large-scale industrial production.
In the prior art, there is no process for separating and purifying cichoric acid from Echinacea purpurea extract by non-column chromatography

Method used

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  • Method for non column chromatography separation and purification of witloof acid from Echinacea purpurea extractive
  • Method for non column chromatography separation and purification of witloof acid from Echinacea purpurea extractive

Examples

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Effect test

Embodiment 1

[0014] (1) Dissolution extraction process:

[0015] Get 3g3.6% cichoric acid extract, add 50ml extraction solvent, the extraction solvent of the present embodiment is acetonitrile: water=1:4, adjust pH with a small amount of acid to be 4, ultrasonic extraction 30min, under the regulation of 10000rpm centrifugal 5min, The supernatant can be obtained, and the one-time extraction efficiency is above 98%.

[0016] (2) Allocation enrichment process:

[0017] Measure 40ml of the supernatant, add 8g of anhydrous magnesium sulfate and 2g of sodium chloride, stir, and ultrasonicate for 2 minutes to promote the dissolution of the salt. The original homogeneous solution gradually appears stratified. Centrifuge at 10,000rpm for 5min to obtain two layers with clear boundaries. . Wherein the volume of the upper layer solution where cichoric acid is located is about 4ml, accounting for 1 / 10 of the volume of the original solution, and the recovery rate of cichoric acid in this step is 85%. ...

Embodiment 2

[0021] (1) Dissolution extraction process:

[0022] Get the cichoric acid extract of 100g4%, add 1100ml extraction solvent; The extraction solvent of the present embodiment is acetone: water=1:2,

[0023] Use formic acid to adjust the pH to about 3, ultrasonically extract for 30 minutes, and centrifuge at 10,000 rpm for 5 minutes to obtain the supernatant, and the extraction efficiency is above 95%.

[0024] (2) Allocation enrichment process:

[0025] Take 1100ml of supernatant, add 120g of dipotassium hydrogen phosphate and 60g of sodium chloride, stir, and ultrasonically promote the dissolution of the salt. The original homogeneous solution gradually becomes stratified. Centrifuge at 10,000rpm for 5min to obtain two layers with clear boundaries. Wherein the volume of the upper layer solution where cichoric acid is located is 130ml.

[0026] (3) Drying and purification process:

[0027] Take 130ml of the upper layer solution, add 300ml of chloroform and absolute ethanol (v...

Embodiment 3

[0029] (1) Dissolution extraction process:

[0030] Get the cichoric acid extract of 1000g4.5%, add the mixture of 20000ml ethanol and water, the extraction solvent of the present embodiment is ethanol: water=1:2,

[0031] Use 170ml of formic acid to adjust the pH to about 2, ultrasonically extract for 30 minutes, and centrifuge at 10,000rpm for 5 minutes to obtain the supernatant, and the extraction efficiency is above 95%.

[0032] (2) Allocation enrichment process:

[0033] Take 20,000ml of supernatant, add 3,000g of ammonium sulfate and 750g of potassium chloride, stir, and ultrasonically promote the dissolution of the salt. The original homogeneous solution gradually becomes stratified. Centrifuge at 10,000rpm for 5min to obtain two layers with clear boundaries. Wherein the volume of the upper layer solution where cichoric acid is located is 2500ml.

[0034] (3) Drying and purification process:

[0035] Get 2500ml upper layer solution, add 5000ml chloroform and dehydra...

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Abstract

The invention discloses a method for non column chromatography separation and purification of witloof acid from an Echinacea purpurea extractive. The method comprises the following steps: adding an extract solvent in 3-5% of weighed Echinacea purpurea extractive, and adding acid to regulate the pH to 2-4, carrying out ultrasonic extraction, and centrifuging so as to obtain supernate; adding 0.1-0.3g of inorganic mixed salt in each milliliter of supernate; stirring, carrying out ultrasonic dissolution, and centrifuging so that the solution is divided into upper and lower phases, the volume ratio of the upper phase to the lower phase is 1:(8-12), and the witloof acid is distributed on the upper phase, thereby achieving the separation and enrichment of the witloof acid; and adding chloroformand absolute ethyl alcohol in the upper phase solution for decompression evaporation so as to obtain a deep yellow powder with 25-40% of witloof acid, wherein the volume of the chloroform and absolute ethyl alcohol is 2-3 times as much as that of the upper phase solution. By using the method in the invention, the purity of the witloof acid is improved by almost 11 times as compared with that of the witloof acid in the raw material, thereby effectively reducing the cost. The used organic solvent and salt can be recycled, thereby effectively saving the cost.

Description

technical field [0001] The present invention relates to a method for purifying and preparing cichoric acid from Echinacea purpurea extract. In particular a method for the non-column chromatographic separation and purification of cichoric acid from Echinacea purpurea extracts. Background technique [0002] The main components of Echinacea purpurea include caffeic acid derivatives, alkylamines and polysaccharides. According to research, cichoric acid in caffeic acid derivatives has obvious immune regulation function, can degrade free radicals, inhibit HIV-1 integrase, and promote T cell production. Protect cells infected by HIV-1 and other functions. Therefore, cichoric acid has become the object of people's scrambling research, and has become a kind of immunostimulator and immunomodulator that has attracted much attention in the world. Its pharmaceutical preparations have been widely popular in North America, Europe and Australia. At present, in my country, there has been l...

Claims

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Application Information

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IPC IPC(8): C07C69/732C07C67/58
Inventor 陈波李圣军
Owner HUNAN NORMAL UNIVERSITY
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