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Method for separating and purifying mangiferin from mango pericarp

A technology for separation and purification of mangiferin, which is applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., can solve the problems of unreported, unguaranteed purity of mangiferin products, extensive process, etc., and achieve high purity and production The process is safe and easy to operate, and the production cycle is short

Active Publication Date: 2012-08-01
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the existing raw materials for extracting and purifying mangiferin are concentrated in medicinal materials and mango leaves. Most of the technical methods use lye extraction or a certain concentration of alcohol extraction combined with crystallization to obtain mangiferin. However, these processes are relatively extensive, and the purity of the obtained mangiferin products cannot be guaranteed.
[0005] In recent years, the extraction and purification of high-purity natural products with macroporous resin combined with high-speed countercurrent chromatography has been successful in many aspects. research has not been reported

Method used

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  • Method for separating and purifying mangiferin from mango pericarp
  • Method for separating and purifying mangiferin from mango pericarp
  • Method for separating and purifying mangiferin from mango pericarp

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1 The present invention carries out the screening determination of influence factor by following test

[0023] 1. Selection of purification materials

[0024] Freeze-dried ‘Machesu’ mango fruit materials, including pericarp, pulp, seed coat, and seed kernel, are crushed into fine powder with a mill. Accurately weigh a certain amount of freeze-dried powder, soak in the extract solution (methanol:ethanol:acetone 1:1:1, v / v / v) for 2 hours (solid-liquid ratio 1:20), ultrasonically extract twice, and centrifuge at 10,000 rpm After 10 min, the combined supernatants were used for HPLC analysis of mangiferin. HPLC mobile phase consisted of 2% acetic acid (A) and 0.5% acetic acid:chromatographic acetonitrile (1:1, v / v) (B) with 0-2 min: 95% A, 2-10 min: 95-75% A , 10-40 min: 75-45% A, 40-45 min: 45-10% A, 45-50min: 10-45% A, 50-55 min: 45-95% A, 55-60 min: 95 % A gradient elution, the flow rate was 0.6 ml / min, the stationary phase was Waters C18 column, the column ...

Embodiment 2

[0043] The operation method of separating and purifying mangiferin of the present invention is carried out according to the following steps:

[0044] see figure 1 , (1) Weigh 10 g of 'Lvpimang' pericarp, add 200 ml of extract solution (methanol: ethanol: acetone 1:1:1, v / v / v), soak for 2 h, sonicate for 30 min, filter to get the supernatant , add 200 ml of extract to the filter residue, sonicate for 30 min, filter, combine the two supernatants, evaporate at 45°C to the extract, dissolve the extract in double distilled water to obtain 210 ml of crude extract;

[0045] (2) 210 ml (0.35 mg / ml mangiferin) crude extract, extracted twice with equal volume of ethyl acetate, concentrated the ethyl acetate phase and then extracted once with water, combined the lower phases with rotary evaporation at 45°C to remove the ethyl acetate to obtain 207 ml aqueous extract;

[0046] (3) 207 ml (0.25 mg / ml mangiferin) was injected into HPD100 macroporous resin (20 ml) at a flow rate of 2 ml / m...

Embodiment 3

[0049] The operation method of separating and purifying mangiferin of the present invention is carried out according to the following steps:

[0050] see figure 1 , (1) Weigh 10 g of 'Liuxiangmang' mango skin, add 200 ml of petroleum ether to soak for 2 h, ultrasonicate for 30 min, filter to remove the petroleum ether layer, and add 200 ml of extract (methanol : ethanol: acetone 1:1:1, v / v / v), sonicate for 30 min, filter to get the supernatant, add 200 ml extract solution to the filter residue, sonicate for 30 min, filter, combine the two supernatants, and evaporate at 45°C To the extract, dissolve the extract in double distilled water to obtain 235 ml crude extract;

[0051] (2) 235 ml (0.15 mg / ml mangiferin) crude extract, extracted twice with equal volume of ethyl acetate, concentrated the ethyl acetate phase and then extracted once with water, combined the lower phases with rotary evaporation at 45°C to remove the ethyl acetate to obtain 188 ml aqueous extract;

[0052...

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Abstract

The invention provides a method for effectively separating and purifying mangiferin from mango pericarp. According to the method, the liquid-liquid extraction, a macroporous resin and HSCCC (High-Speed Counter Current Chromatography) coupling technique is adopted, and dried mango pericarp powder is used as the raw material, extracted with ethyl acetate, and separated and purified by HPD100 macroporous resin and HSCCC to obtain high-purity mangiferin. According to the invention, the method is reasonable in design, simple in operation, safe in production flow, easy in operation, short in production period, low in sample consumption and low in equipment investment; the whole purifying process is accurately quantified by HPLC (High-Performance Liquid Chromatography), so that the accuracy is high, and the conditions are stable and easy to control; the solvent used by HSCCC can be recycled, so that the cost is lower; the purified product is high in recovery rate and purity, and the purity of the finally purified mangiferin is not less than 98%; and the method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of extraction, separation and purification of natural compounds, and specifically relates to a method for separating and purifying mangiferin by using mango peel as a raw material, liquid-liquid extraction, macroporous resin and HSCCC combined technology. Background technique [0002] Mangiferin (mangiferin), alias mangiferin, Guan Zhi Mu Ning, molecular formula: C 19 h 18 o 11 , Molecular weight: 422.34, CAS No.: 4773-96-0, is a carbon glycoside of tetrahydroxypyridine, which belongs to the biphenylpyrazone compounds. Mangiferin exists in Anacardiaceae mango ( Mangifera indica L.) fruits, leaves, bark, Liliaceae Anemarrhena ( Anemarrhena asphodeloides Bge.) rhizomes, aerial parts, Iridaceae plants shoot dry [ Belamcanda chinensis (L.) DC.] flowers, leaves and other plants. The structural formula of mangiferin is as follows: [0003] [0004] Recent studies have shown that mangiferin has strong a...

Claims

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Application Information

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IPC IPC(8): C07H17/04C07H1/08
Inventor 李鲜孙崇德罗丰雷陈昆松
Owner ZHEJIANG UNIV
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