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Method for extracting high-purity licochalcone A

A technology of licorice chalcone and extraction method, which is applied in the field of separation and purification of natural substances, can solve the problems of high maintenance cost, high price, and high cost, and achieve the effect of low equipment requirements, cheap raw and auxiliary materials, and easy amplification

Pending Publication Date: 2021-08-03
NANJING POLYTECHNIC INSITUTE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The current methods include "Separation and Purification of Glycyrrhizalcone A and Pachychalcone A by High Speed ​​Countercurrent Chromatography" by Wang Qiao'e, Modern Chinese Medicine Research and Practice, 2004, "Research on the Separation and Purification Process of Glycyrrhizalcone" by Wang Shujie, Ningxia Engineering Technology, 2005, "Separation, Structure and Total Synthesis of Licochalcone" by Xu Rensheng, Acta Chemicals, 1979, etc., and patents CN102010313A, CN2007100525211 and CN105859538A all have related reports on the extraction of licochalcone A, or the cost is too high High, complex equipment, only suitable for experimental research stage, or the purity is not high enough
Wherein CN105859538A adopts supercritical extraction, the equipment is expensive, the maintenance cost is high, and it is not suitable for large-scale production
CN2007100525211 The filler polyamide and dextran gel used for purification are expensive, several to tens of times that of silica gel, and the highest purity is only 93%, which is far from the standard for medicinal use

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A method for extracting high-purity licorice chalcone A. Take 10 kg of licorice root and add 70 L of methanol to reflux, extract three times, combine the extracts and concentrate under pressure to obtain a black paste; add water to disperse the paste, and extract with chloroform for 4 Once, the extracts were combined and evaporated to dryness to obtain the crude product; the crude product was subjected to silica gel column chromatography, and the mixed solvent petroleum ether: ethyl acetate=10:1~1:1 (volume ratio) was eluted, and the part A of licochalcone was collected and evaporated. Dried to obtain an orange solid with a purity of 98.3%; recrystallized from ethanol to obtain 25.1 g of orange needles with a purity of 99.5%.

Embodiment 2

[0021] A method for extracting high-purity licorice chalcone A. Take 10 kg of licorice and add 10 L of ethanol to heat and reflux, extract three times, combine the extracts and concentrate under pressure to obtain a black paste; add water to disperse the paste, and extract with ethyl acetate for 3 time, combine the extracts, and evaporate to dryness to obtain the crude product; neutral alumina on the crude product, mixed solvent petroleum ether: ethyl acetate=20:1~1:1 (volume ratio) elution, collect licochalcone A part, evaporate Dried to obtain an orange solid with a purity of 98.4%; recrystallized from ethanol to obtain 24.8 g of orange needles with a purity of 99.7%.

Embodiment 3

[0023] A method for extracting high-purity licorice chalcone A. Take 10 kg of licorice and add 70 L of methanol to heat and reflux, extract three times, combine the extracts and concentrate under pressure to obtain a black paste; add water to disperse the paste, and extract with dichloromethane for 4 The second time, the combined extracts were evaporated to dryness to obtain the crude product; the crude product was subjected to silica gel column chromatography, and the mixed solvent dichloromethane:methanol=100:1~30:1 (volume ratio) was eluted, and part A of licochalcone was collected and evaporated to dryness An orange solid was obtained with a purity of 98.1%; methanol recrystallized to obtain 25.1 g of orange needle crystals with a purity of 99.3%.

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PUM

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Abstract

The invention discloses a method for extracting high-purity licochalcone A. The method belongs to the field of separation and purification of natural substances, and comprises the following steps of crushing liquorice, extracting with a solvent for multiple times, concentrating and evaporating an extracting solution to dryness, adding water into an obtained crude product, dispersing, extracting with a solvent, evaporating an extracting solution to dryness, separating with a column, and collecting a licochalcone A part, and drying by distillation to obtain high-purity licochalcone A with the purity of 98%, and recrystallizing to obtain licochalcone A with the purity of 99% or above. The process is simple, the solvent can be recycled and reused, the cost is low, the purity is high, and industrial production is easy.

Description

technical field [0001] The invention belongs to the field of separation and purification of natural substances, in particular to a method for extracting high-purity licochalcone A. Background technique [0002] Licorice is the dried root and rhizome of Glycyrrhiza uralensis Fisch., Glycyrrhiza inflata Bat. or Glycyrrhiza glabra L., a leguminous plant. It contains a large amount of phenolic components, licochalcone A (Licochalcone A) is a phenolic chalcone compound present in licorice. Clinical and pharmacological studies have shown that licochalcone A has antioxidant, anti-inflammatory, antibacterial, anti-tumor, anti-leishmaniasis, Immunopromoting and estrogen-like activities have broad application prospects in clinical practice. [0003] The current methods include "Separation and Purification of Glycyrrhizalcone A and Pectin A by High-speed Countercurrent Chromatography" by Wang Qiao'e, Modern Chinese Medicine Research and Practice, 2004, "Research on the Separation and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/84C07C45/80C07C45/82C07C45/79
CPCC07C45/80C07C45/82C07C45/79C07C49/84
Inventor 李冰峰常思源宋伟钟开龙刘蕾武亚明
Owner NANJING POLYTECHNIC INSITUTE
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