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Method for preparing high-purity arundoin

A high-purity technology of arunecillin, which is applied in the field of separation of effective components of natural plants, can solve the problems of extraction process reports on the pharmacological effects of arunecilin, and the lack of arunecilin, and achieve large preparation, short separation time, and high product purity Effect

Inactive Publication Date: 2011-11-23
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are few studies on Arunin, and there is no report on the pharmacological effects of Arunin and its extraction process.

Method used

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  • Method for preparing high-purity arundoin

Examples

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Comparison scheme
Effect test

Embodiment 1

[0012] Grind 1.5kg of the rhizome of Imperatae Rhizoma, soak in 80% ethanol at 60°C for 0.5 hour, reflux extraction for 2 hours, extract twice, combine the extracts, concentrate the extracts under reduced pressure to obtain an ethanol extract. The ethanol extract was extracted with chloroform, and the chloroform layer was concentrated under reduced pressure to obtain 8.7 g of extract. The chloroform extract was subjected to silica gel column chromatography, chloroform-acetone (1:1.5) isocratic gradient elution, the eluate flowing out in 2-4 column bed volumes was collected, the solvent was recovered, and crystallized with chloroform-acetone to obtain Coarse crystal 5.3g. 200 mg of crystals were separated by high-speed countercurrent chromatography, and the solvent system n-hexane-ethyl acetate-methanol-water was selected. First, the above-mentioned solvent system was configured in a separatory funnel at a volume ratio of 8:2:1.5:0.5, and shaken well After standing for stratif...

Embodiment 2

[0014] Grind 1.5 kg of Rhizoma Imperatae medicinal material, soak in 95% ethanol at 60°C for 0.5 hour, reflux extraction for 1.5 hour, extract twice, combine extracts, concentrate under reduced pressure to obtain ethanol extract. The ethanol extract was extracted with chloroform, and the chloroform layer was concentrated under reduced pressure to obtain 8.5 g of extract. The chloroform extract was subjected to silica gel column chromatography, chloroform-acetone (1:1.5) isocratic gradient elution, the eluate flowing out in 2-4 column bed volumes was collected, the solvent was recovered, and crystallized with chloroform-acetone to obtain Coarse crystal 5.0g. 200 mg of crystals were separated by high-speed countercurrent chromatography, and the solvent system n-hexane-ethyl acetate-methanol-water was selected. First, the above-mentioned solvent system was arranged in a separatory funnel at a volume ratio of 10:5:2.5:1, and shaken evenly After standing for stratification, separa...

Embodiment 3

[0016] Grind 1.5 kg of Rhizoma Imperatae medicinal material, soak in 85% ethanol at 60°C for 0.5 hour, reflux extraction for 1.5 hour, extract twice, combine extracts, concentrate extracts under reduced pressure to obtain ethanol extract. The ethanol extract was extracted with chloroform, and the chloroform layer was concentrated under reduced pressure to obtain 8.4 g of extract. The chloroform extract was subjected to silica gel column chromatography, chloroform-acetone (1:1.5) isocratic gradient elution, the eluate flowing out in 2-4 column bed volumes was collected, the solvent was recovered, and crystallized with chloroform-acetone to obtain Coarse crystal 5.1g. 250 mg of crystals were separated by high-speed countercurrent chromatography, and the solvent system n-hexane-ethyl acetate-methanol-water was selected. First, the above-mentioned solvent system was arranged in a separatory funnel at a volume ratio of 13:3.5:4:2, and shaken well After standing for stratification,...

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Abstract

The invention provides a method for preparing high-purity arundoin. The method provided by the invention comprises the following steps of: crushing cogongrass rhizome and leaching by using an ethanol solution; decompressing and concentrating to obtain an ethanol extractive; extracting the ethanol extractive through utilizing trichloromethane and carrying out a chromatography on a decompressed and concentrated trichloromethane layer through utilizing a silica gel column; eluting by using trichloromethane-acetone and collecting eluent flowing from 2-4 column bed volumes; decompressing and concentrating the eluent and then standing and crystallizing; filtering the crystal, separating by taking n-hexane-ethyl acetate-methanol-water as a solvent system and utilizing a high-speed countercurrent chromatography, and detecting by an ultraviolet detector; collecting fluid and recycling reagents; and then re-crystallizing by using methanol and drying to obtain the product. The method provided by the invention is used for purifying the arundoin; and the method has the advantages of simple and easily-operated process, high efficiency and high product content so that the method is suitable for the industrial preparation.

Description

Technical field: [0001] The invention belongs to the field of separation of effective components of natural plants, and relates to a preparation method of high-purity arundin. Background technique: [0002] Arundoin, also known as Arundoin, containing Arundoin, molecular formula C 31 h 52 O:, the molecular weight is 440.751, and the structural formula is: [0003] [0004] The rhizome of Imperata koenigii (Retz.) Beauv. is the rhizome of Grass plant Imperata koenigii (Retz.) Beauv. It has the functions of cooling blood, stopping bleeding, clearing heat and diuresis. At present, there are few studies on arunecillin, and there is no report on the pharmacological effects of arunecilin and its extraction process. Invention content: [0005] The purpose of the present invention is to provide a method for preparing high-purity arundin. [0006] Technical scheme of the present invention is as follows: [0007] A preparation method of high-purity arundin, which is characte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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