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A kind of preparation method of medicinal chlorogenic acid

A chlorogenic acid and sample technology, applied in the field of preparation of medicinal chlorogenic acid, can solve the problems of high price, high cost, troublesome operation and the like, and achieve the effect of simple operation and low cost

Active Publication Date: 2016-01-06
SICHUAN JIUZHANG BIO TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Resin column chromatography, this method can enrich and purify chlorogenic acid, but this method alone cannot make the sample purity and impurities meet the pharmaceutical requirements; polyamide column chromatography, this method can obtain chlorogenic acid and flavonoids Very good separation, can be purified to obtain higher purity chlorogenic acid, but the operation is troublesome, the elution time is long, the cost is high, the material is not easy to regenerate, and the industrialization investment is large; Gel chromatography can obtain high purity by this method Chlorogenic acid, but because the gel is expensive and the product yield is low, it is difficult to realize industrial production; high-performance liquid chromatography, this method can obtain relatively high-purity chlorogenic acid, but due to high technical requirements and low yield, currently Still in the laboratory stage; crystallization and recrystallization are commonly used refining methods, which can enrich and purify high-purity chlorogenic acid, but usually a single solvent is used for crystallization and recrystallization purification, and the impurities removed by purification are highly targeted , it is impossible to separate and purify impurities of different polarities at the same time, the selectivity of the extract is relatively high, and it cannot be widely used in extracts prepared by different processes
There are some research literature reports that using complex solvent crystallization and recrystallization refining methods, by changing the type and ratio of complex solvents to remove impurities of different polarities to achieve the purpose of purification, this method can effectively remove impurities of different polarities in the extract , but due to the great difficulty in recycling and reusing the composite solvent, there are also certain limitations. At the same time, there is a great potential safety hazard due to the residual composite solvent in the product

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  • A kind of preparation method of medicinal chlorogenic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1 The preparation method of medicinal chlorogenic acid of the present invention

[0024] 1. Sample aqueous phase treatment: Prepare the sample with purified water to prepare a solution containing 500 mg / ml of chlorogenic acid, and filter; the sample is extracted from Eucommia leaves to obtain an extract with a chlorogenic acid content of 90%; the preparation temperature is 40 ℃.

[0025] 2. Freezing: Freeze the filtered filtrate below 0°C until the filtrate is completely frozen;

[0026] 3. Thawing and filtering: thaw the frozen ice cubes at 25°C, and keep the temperature of the thawing liquid not higher than 5°C, then filter;

[0027] 4. Organic phase treatment of the filter residue: fully dissolve the filtered residue with an organic solvent, and filter; the organic solvent is ethyl acetate; the dissolution temperature is 60°C;

[0028] 5. Concentration and crystallization: Concentrate the organic solution under low temperature and negative pressure until...

Embodiment 2

[0030] Embodiment 2 The preparation method of medicinal chlorogenic acid of the present invention

[0031] 1. Sample aqueous phase treatment: Prepare the sample with purified water to make a solution containing 800 mg / ml chlorogenic acid, and filter; the sample is extracted from Eucommia leaves to obtain an extract with a chlorogenic acid content of 60%; the preparation temperature is 50 ℃;

[0032] 2. Freezing: Freeze the filtered filtrate below 0°C until the filtrate is completely frozen;

[0033] 3. Thawing and filtering: thaw the frozen ice cubes at 10°C, and keep the temperature of the thawing liquid not higher than 5°C, then filter;

[0034] 4. Treatment of the organic phase of the filter residue: fully dissolve the filtered residue with an organic solvent, and filter; the organic solvent is propyl acetate; the dissolution temperature is 60°C;

[0035] 5. Concentration and crystallization: Concentrate the organic solution under low temperature and negative pressure unt...

Embodiment 3

[0038] Embodiment 3 The preparation method of medicinal chlorogenic acid of the present invention

[0039] 1. Sample aqueous phase treatment: prepare the sample with purified water to prepare a solution containing chlorogenic acid 20mg / ml, and filter; the sample is extracted from Eucommia leaves to obtain an extract with a chlorogenic acid content of 85%; the preparation temperature is 20 ℃;

[0040] 2. Freezing: Freeze the filtered filtrate below 0°C until the filtrate is completely frozen;

[0041] 3. Thawing and filtering: thaw the frozen ice cubes at 5°C, and keep the temperature of the thawing liquid not higher than 5°C, then filter;

[0042] 4. Treatment of the organic phase of the filter residue: fully dissolve the filtered residue with an organic solvent, and filter; the organic solvent is methyl acetate; the dissolution temperature is 20°C;

[0043] 5. Concentration and crystallization: Concentrate the organic solution under low temperature and negative pressure unt...

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Abstract

The invention provides a preparation method of medicinal chlorogenic acid, wherein the preparation method comprises the following steps: a, carrying out water phase treatment on a sample; b, freezing; c, thawing and filtering; d, carrying out organic phase treatment on the filter residue; e, concentrating and crystallizing; f, according to a difference of the contents of chlorogenic acid in the sample, selecting the repeating times of the a-e steps; and g, drying. A chlorogenic acid extract is separated and purified by the method, water-soluble impurities and fat-soluble impurities in the extract can be better removed, and thus the impurity content of the final product meets the medicinal requirements; at the same time, the method has the advantages of simple operation, recyclable organic solvent and low cost, is suitable for further separation and purification of a chlorogenic acid extract extracted by all kinds of methods, and is especially suitable for the preparation of the medicinal chlorogenic acid.

Description

technical field [0001] The invention relates to a preparation method of medicinal chlorogenic acid. Background technique [0002] Chlorogenic acid has a wide range of antibacterial effects, but it can be inactivated by proteins in the body. Similar to caffeic acid, it can increase the central excitability of rats when taken orally or intraperitoneally. It can increase the intestinal motility of rats and mice and the tension of rat uterus. Good choleretic effect, can enhance the secretion of bile in rats. It is sensitizing to humans, and after inhalation of plant dust containing this product, asthma and dermatitis may occur. At present, there are many separation and purification methods of chlorogenic acid reported, such as: application number: CN201010558366 Invention name: a production method for preparing chlorogenic acid by freezing and concentrating crystallization, the present invention discloses a production method for chlorogenic acid crystallization, which belongs...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/732C07C67/48C07C67/52
CPCC07C67/48C07C67/52C07C69/732
Inventor 张洁张亮黄望
Owner SICHUAN JIUZHANG BIO TECH CO LTD
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