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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  • Abstract
  • Description
  • Claims
  • Application Information

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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 th

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

Experimental program
Comparison scheme
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Example Embodiment

[0013] Example 1:

[0014] (1) Dissolution and extraction process:

[0015] Take 3g 3.6% cichoric acid extract, add 50ml extraction solvent, the extraction solvent in this example is acetonitrile: water=1:4, adjust pH to 4 with a small amount of acid, ultrasonic extraction for 30min, centrifuge at 10000rpm for 5min, The supernatant can be obtained, and the one-time extraction efficiency is above 98%.

[0016] (2) Distribution and enrichment process:

[0017] Measure 40ml of supernatant, add 8g of anhydrous magnesium sulfate and 2g of sodium chloride, stir and ultrasonic for 2min to promote salt dissolution. The original homogeneous solution gradually appears layered. Centrifuge at 10000rpm for 5min to obtain two layers with obvious boundaries . The volume of the upper layer solution where cichoric acid is located is about 4ml, which accounts for about 1 / 10 of the volume of the original solution. The recovery rate of cichoric acid in this step is 85%.

[0018] (3) Drying and purificat...

Example Embodiment

[0020] Example 2:

[0021] (1) Dissolution and extraction process:

[0022] Take 100g of 4% cichoric acid extract and add 1100ml extraction solvent; the extraction solvent in this example is acetone:water=1:2,

[0023] Adjust the pH to about 3 with formic acid, ultrasonically extract for 30 minutes, and centrifuge at 10000 rpm for 5 minutes to obtain the supernatant. The extraction efficiency is above 95%.

[0024] (2) Distribution and enrichment process:

[0025] Take 1100ml of supernatant, add 120g of dipotassium hydrogen phosphate and 60g of sodium chloride, stir, ultrasound to promote the dissolution of the salt, the original homogeneous solution gradually appears layering, centrifugation at 10000rpm for 5min, obtain two layers with obvious boundaries. The volume of the upper solution where cichoric acid is located is 130 ml.

[0026] (3) Drying and purification process:

[0027] Take 130ml of the upper layer solution, add 300ml of chloroform and absolute ethanol (volume ratio is 1:3...

Example Embodiment

[0028] Example 3:

[0029] (1) Dissolution and extraction process:

[0030] Take 1000 g of 4.5% cichoric acid extract and add 20000 ml of a mixture of ethanol and water. The extraction solvent in this example is ethanol:water=1:2.

[0031] Adjust the pH to about 2 with 170ml of formic acid, ultrasonically extract for 30min, and centrifuge at 10000rpm for 5min to obtain the supernatant. The extraction efficiency is above 95%.

[0032] (2) Distribution and enrichment process:

[0033] Take 20000ml supernatant, add 3000g ammonium sulfate and 750g potassium chloride, stir and ultrasonic to promote the dissolution of the salt, the original homogeneous solution gradually appears layering, centrifugation at 10000rpm for 5min, two layers with obvious boundaries are obtained. The volume of the upper solution where cichoric acid is located is 2500ml.

[0034] (3) Drying and purification process:

[0035] Take 2500ml of the upper solution, add 5000ml of chloroform and absolute ethanol (volume ratio...

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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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