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Preparation method of high-purity mangiferin crystals

A mangiferin and crystallization technology, which is applied in the field of plant extraction, can solve the problems of hard cell wall of dry products, affecting the extraction rate and high production cost, and achieves the effects of easy industrial production, good repeatability and simple method.

Active Publication Date: 2020-07-17
ANALYSIS & TESTING CENT CHINESE ACADEMY OF TROPICAL AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The dry product has a hard cell wall, which affects the extraction rate
[0005] (2) Organic solvent recrystallization method This method is simple to operate and does not require special equipment, but the purity of mangiferin reported in existing patents is mostly lower than 98%, and only a few cases have reached 98%
[0006] (3) Macroporous adsorption resin and gel column chromatography purification method. This method has poor reproducibility, and expensive gel Sephadex LH~20 is used in some patents.
[0007] (4) High performance countercurrent chromatography (HSCCC) purification method This method requires special equipment
[0008] In summary, in the existing patents, the purity of the mangiferin prepared by most of the processes is low (≤98%), or the purity is not clear because the purity analysis is not carried out; structure characterization and principal component analysis of the product, the structure of mangiferin is not clear; while high performance counter-current chromatography, gel column chromatography, etc. have high production costs or poor process repeatability and are not suitable for large-scale production.

Method used

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  • Preparation method of high-purity mangiferin crystals
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  • Preparation method of high-purity mangiferin crystals

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] A preparation method for high-purity mangiferin crystals, comprising the following steps:

[0042] S1. Mangiferin extract: Take fresh mango skin and mango leaves, crush them, and use 2 times the amount of alcohol solution to ultrasonically extract twice, each time for 20 minutes; combine the extracts, filter, and concentrate under reduced pressure to obtain mangiferin extract;

[0043] S2. Crude mangiferin crystallization: extract the mangiferin extract 4 times with 1 times the amount of ethyl acetate, remove the ethyl acetate layer, then extract 4 times with 1 times the amount of mangiferin extract with petroleum ether, and remove the petroleum ether layer , to obtain the mangiferin extract after impurity removal and decolorization, place it in a constant temperature water bath at 40°C to evaporate the solvent, place it in a hot air drying oven at a constant temperature of 40°C for 24 hours, and obtain the crude mangiferin crystals;

[0044] S3. Mangiferin redissolutio...

Embodiment 2

[0047] A preparation method for high-purity mangiferin crystals, comprising the following steps:

[0048] S1. Mangiferin extract: take fresh mango skin and mango leaves, crush them, and use 4 times the amount of alcohol solution to ultrasonically extract 4 times, each time for 40 minutes; combine the extracts, filter, and concentrate under reduced pressure to obtain mangiferin extract;

[0049] S2. Crude mangiferin crystallization: extract the mangiferin extract twice with 3 times the amount of ethyl acetate, remove the ethyl acetate layer, then extract twice with 3 times the amount of mangiferin extract petroleum ether, and remove the petroleum ether layer , to obtain the mangiferin extract after impurity removal and decolorization, place it in a 70°C constant temperature water bath to evaporate the solvent, place it in a hot air drying oven at a constant temperature of 70°C for 36 hours, and obtain the crude mangiferin crystals;

[0050] S3. Mangiferin redissolution: take th...

Embodiment 3

[0053] A preparation method for high-purity mangiferin crystals, comprising the following steps:

[0054] S1. Mangiferin extract: Take fresh mango skin and mango leaves, crush them, and use 2 times the amount of alcohol solution to ultrasonically extract 3 times, each time for 20 minutes; combine the extracts, filter, and concentrate under reduced pressure to obtain mangiferin extract;

[0055] S2. Crude mangiferin crystallization: extract the mangiferin extract three times with 1 times the amount of ethyl acetate, remove the ethyl acetate layer, then extract 3 times with 1 times the amount of mangiferin extract with petroleum ether, and remove the petroleum ether layer , to obtain the mangiferin extract after impurity removal and decolorization, place it in a constant temperature water bath at 40°C to evaporate the solvent, place it in a hot air drying oven at a constant temperature of 40°C for 24 hours, and obtain the crude mangiferin crystals;

[0056] S3. Mangiferin rediss...

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PUM

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Abstract

The invention provides a preparation method of high-purity mangiferin crystals. The method comprises the following steps: preparing mangiferin extract, preparing a mangiferin crystal crude product; redissolving the mangiferin; and recrystallizing the mangiferin; according to the invention, fresh leaves and mango peel are used as raw materials to prepare mangiferin, the loss of the mangiferin caused by degradation, oxidation and the like in the drying process of drying mango leaves and mango peels in the sun or in the drying process can be prevented, the purity of the mangiferin prepared afterrecrystallization is high and reaches 99.84%, the recrystallization method is simple, special instruments and equipment are not needed, the repeatability is good, and industrial production is easy.

Description

technical field [0001] The invention relates to the field of plant extraction, in particular to a method for preparing high-purity mangiferin crystals. Background technique [0002] Mangiferin (mangiferin) is a carbon ketone glycoside of tetrahydroxypyrrole, molecular formula C 19 h 18 o 11 , the structural formula is shown in formula 1, and it is widely found in many plants such as mango, anemarrhena, capillary, and waterweed. In the Chinese Pharmacopoeia and the quality standards of various Chinese medicinal materials and Chinese patent medicines, mangiferin is widely used as a quality control indicator. Modern medical research has proved that mangiferin has various pharmacological effects such as anti-oxidation, anti-inflammation, anti-radiation, prevention and treatment of skin aging, lowering blood sugar, lowering uric acid, anti-tumor, and immune regulation, and has a very high development and utilization prospect. [0003] At present, the existing preparation meth...

Claims

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Application Information

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IPC IPC(8): C07D407/04
CPCC07D407/04C07B2200/13
Inventor 阳辛凤庞朝海田海张群刘春华
Owner ANALYSIS & TESTING CENT CHINESE ACADEMY OF TROPICAL AGRI SCI
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