Method for separating and purifying mangiferin from aquilaria sinensis leaves

A technology for separation and purification of mangiferin, applied in the direction of organic chemistry, which can solve problems such as complex process operation, low economic benefits, and long production cycle, and achieve the effects of simple process operation, shortened time and cost, and short production cycle

Active Publication Date: 2014-12-17
北京利科德科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] 1. The purity of mangiferin obtained from most processes is low, or there is no exact guarantee of purity;
[0011] 2. Part of the process is complicated to operate, and a large amount of solvent is required for elution, which is easy to cause harm to the operator, and the cost of the solvent is high;
[0012] 3. The preparation cycle of most processes is long, the recovery rate is low, and the economic benefit is low;
[0013] 4. Mangiferin is unstable under acidic or alkaline conditions. If acid extraction or alkaline extraction is used, most mangiferin may be denatured and inactivated during the preparation process;
[0014] 5. Mango leaves are mostly used as raw materials, which are prone to excessive pesticide residues and are unsafe;

Method used

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  • Method for separating and purifying mangiferin from aquilaria sinensis leaves
  • Method for separating and purifying mangiferin from aquilaria sinensis leaves
  • Method for separating and purifying mangiferin from aquilaria sinensis leaves

Examples

Experimental program
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Effect test

Embodiment 1

[0050] Take 30 kg of coarse powder of Akira sinensis leaves and place it in a percolation bucket, add 70% acetone aqueous solution for percolation, receive percolation liquid, combine and concentrate at 45°C under low pressure to 180L. Extract with petroleum ether and n-butanol respectively to obtain 165.2 g of n-butanol part extract. After mixing the sample with normal-phase silica gel, it is separated by normal-phase column chromatography. One column volume is connected as one part, and the received flow After concentration under low pressure, TLC detection was carried out. The fractions mainly containing mangiferin were combined and the solvent was recovered under low pressure at 35° C. to obtain 3.366 g of fractions mainly containing mangiferin. After the combined fractions were mixed with normal phase silica gel, they were separated by normal phase column chromatography, and 1 / 2 column volume was taken as one part. At the same time, the received fractions were concentrate...

Embodiment 2

[0052] Take 60 kg of coarse powder of Akira sinensis leaves in a percolation barrel, add 75% ethanol aqueous solution for percolation, receive percolation liquid, combine and concentrate at 50°C under low pressure to 300L. Use petroleum ether and n-butanol to extract respectively, take 340.7g of n-butanol extract, mix it with normal phase silica gel, and separate it by normal phase column chromatography. After concentration under low pressure, TLC detection was carried out. The fractions mainly containing mangiferin were combined and the solvent was recovered under low pressure at 40° C. to obtain 7.098 g of fractions mainly containing mangiferin. After the combined fractions were mixed with normal phase silica gel, they were separated by normal phase column chromatography, and 1 / 2 of the column volume was taken as one portion. At the same time, the received fractions were concentrated under low pressure and then detected by TLC. The fractions mainly containing mangiferin wer...

Embodiment 3

[0054]Take 90 kg of coarse powder of Akira sinensis leaves in a percolation bucket, add 75% acetone aqueous solution for percolation, receive percolation liquid, combine and concentrate at 45° C. under low pressure to 480 L. Extracted with petroleum ether and n-butanol respectively to obtain 478.2 g of n-butanol extract, which was mixed with normal phase silica gel and separated by normal phase column chromatography. One column volume was connected as one part, and the received flow After concentration under low pressure, TLC detection was carried out. The fractions mainly containing mangiferin were combined and the solvent was recovered under low pressure at 45° C. to obtain 9.998 g of fractions mainly containing mangiferin. After the combined fractions were mixed with normal phase silica gel, they were separated by normal phase column chromatography, and 1 / 2 of the column volume was taken as one portion. At the same time, the received fractions were concentrated under low pr...

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Abstract

The invention discloses a method for separating and purifying mangiferin from aquilaria sinensis leaves. The method is used for solving the problems such as low purity, low yield and complex operation of the mangiferin separated by virtue of the existing process. The method comprises the following step: quickly preparing the high-purity mangiferin by use of the aquilaria sinensis leaves used as raw materials by virtue of adopting a method of combining normal phase column chromatography with high-speed counter-current chromatography. The method has the advantages of great preparation amount, high efficiency, quickness, low cost, simplicity in operation, high product quality and no pollution; and moreover, a solvent can be recycled, the solvent cost and the solvent treatment cost can be lowered, and the method can be widely applied to industrial production.

Description

【Technical field】 [0001] The invention belongs to the field of extraction, separation and purification of natural compounds, and in particular relates to a method for rapidly preparing high-purity compounds by using column chromatography combined with HSCCC technology. 【Background technique】 [0002] Aquilaria sinensis, also known as soil agarwood, agarwood tree, Guanxiang, tooth incense, daughter incense, etc., is a plant of the genus Aquilaria in the family Daphneaceae, an evergreen tree, and is a unique national second-level protected plant in China. In Guangdong, Hainan, It is planted in Guangxi, Fujian and other places, and it is a rare and precious medicinal material commonly used in traditional Chinese medicine. The heartwood of Baimuxiang is pungent, bitter, and slightly warm. It has the effects of lowering Qi, warming the kidneys, and relieving pain. The resin-containing heartwood (commonly known as agarwood) of the tree body can be used as a raw material for spice...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D407/04
CPCC07D407/04
Inventor 梁耀光杨懋勋张天佑
Owner 北京利科德科技有限公司
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