Preparation method of high-purity arctigenin

A technology of arctigenin and arctium fruit, which is applied in the field of preparation of burdock extract, to achieve the effects of reasonable preparation process design, avoiding heat changes, and high hydrolysis efficiency

Inactive Publication Date: 2013-06-12
NANJING HAIYUAN CHINESE HERBAL PIECES CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The latter process conditions include degreasing the medicinal material of Arctium Fructus with an organic solvent, adding snail enzyme to the medicinal material after degreasing to hydrolyze arctiin into arctigenin, then separating by silica gel column chromatography, and purifying by solvent recrystallization to obtain arctigenin crystals. The above two preparation methods The workload is heavy, the preparation efficiency is low, and column chromatography requires a large amount of organic solvents, which is poor in pertinence and high in cost

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  • Preparation method of high-purity arctigenin

Examples

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Embodiment 1

[0024] Take 500g of arctium medicinal material, crush it through an 80-mesh sieve, pack the medicinal material powder into a column, use petroleum ether at 60-90°C to percolate and degrease, and trace the percolation process with a thin-layer spot plate until no spots appear on the spot plate of the petroleum ether percolation liquid. Then use ethyl acetate percolation to extract the active ingredient of arctiin, and trace the percolation process with thin-layer spot plate until no spots appear in the percolation solution of ethyl acetate. The petroleum ether percolation liquid and the ethyl acetate percolation liquid were concentrated under reduced pressure respectively to obtain 200 g of the petroleum ether oil fraction and 30 g of the ethyl acetate fraction, and the pH value of the ethyl acetate fraction was adjusted to 3.0, and then the ethyl acetate fraction was placed at 4 ℃ refrigerator, arctigenin crystals were separated out, the crystals were recrystallized with ethyl ...

Embodiment 2

[0026] Take 2 kg of burdock fruit medicinal material, crush it through an 80-mesh sieve, pack the medicinal material powder into a column, and then use 60-90°C petroleum ether to percolate and degrease, and trace the percolation process by thin-layer spotting until no spots appear on the petroleum ether percolation spot. Then the active ingredient of arctiin was extracted by ethyl acetate percolation, and the percolation process was tracked with a thin-layer spot plate until no spots appeared in the ethyl acetate percolation solution. Concentrate the petroleum ether percolation liquid and ethyl acetate percolation liquid under reduced pressure respectively to obtain 900 g of petroleum ether oil fraction and 140 g of ethyl acetate fraction, adjust the pH value of the ethyl acetate fraction to 3.0, and place the ethyl acetate fraction at 4°C In the refrigerator, arctigenin crystals were precipitated. The crystals were recrystallized with ethyl acetate and purified by high perfor...

Embodiment 3

[0028] Take 5kg of burdock fruit medicinal material, crush it through a 100-mesh sieve, pack the medicinal material powder into a column, and then use 60-90°C petroleum ether to percolate and degrease, and trace the percolation process with a thin-layer spot plate until no spots appear on the spot plate of the petroleum ether percolation liquid. Then use ethyl acetate percolation to extract the active ingredient of arctiin, and trace the percolation process with thin-layer spot plate until no spots appear in the percolation solution of ethyl acetate. The petroleum ether percolation liquid and the ethyl acetate percolation liquid were respectively concentrated under reduced pressure to obtain 3200 g of the petroleum ether oil fraction and 354 g of the ethyl acetate fraction, adjust the pH value of the ethyl acetate fraction to 4.0, and place the ethyl acetate fraction at 4°C In the refrigerator, arctigenin crystals were precipitated. The crystals were recrystallized with ethyl ...

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Abstract

The invention discloses a preparation method of high-purity arctigenin. The preparation method of the high-purity arctigenin does not need a heating return flow method to extract arctigenin constituents, does not need an enzymolysis method and a column chromatography, and directly uses ethyl acetate diacolation to extract arctiin in burdock, the potential of hydrogen (PH) value of a diacolation concentrated solution is adjusted to be 3.0-4.0, the arctiin is directly hydrolyzed to become an arctigenin crude product, and an opposite phase preparative liquid chromatography optimized by a large number of experiments is adopted to obtain the high-purity arctigenin. The preparation method of the high-purity arctigenin is reasonable and in the entire preparation process design, high in preparation efficiency, strong in operability, and suitable for industrialized mass production.

Description

technical field [0001] The invention relates to a preparation method of burdock extract, in particular to a preparation method of arctigenin. Background technique [0002] Arctigenin, chemical name: (3R,4R)-[(3,4-Dimethoxyphenyl)methy]dihydro-3-[(4-hydroxy-3-methoxyphenyl)methyl]-2(3H)-furanone, molecular formula: C 21 h 24 o 6， Molecular weight: 372.41 [0003] Molecular Structure: [0004] [0005] It has been reported recently that arctigenin has shown strong pharmacological activities in anti-inflammatory, anti-virus, anti-tumor, immune regulation, etc.; at the same time, it can be used as a new type of heat shock response inhibition regulator, which can treat cancers that are overheated. Treatment can help. In addition, it also has the effect of anti-senile dementia and the effect of inhibiting K+ contracture. [0006] Arctigenin is a lignan compound, mainly derived from Arctium lappa L., the fruit of Arctium lappa L. It is recorded in the previous editions ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/33
Inventor 蔡宝昌刘启迪秦昆明周树云王玉陈毅沈保家
Owner NANJING HAIYUAN CHINESE HERBAL PIECES CO LTD
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