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Method for gathering and purifying agrimonine in agrimony

A technology of agrimonin and Agrimony, which is applied to the preparation of Agrimin in the enrichment and purification of Agrimony by high-speed countercurrent chromatography separation method, and the field of purification of Agrimony, which can solve the problems of low extraction rate and low extraction purity, Achieve high recovery rate, no sample loss, and mild separation environment

Inactive Publication Date: 2010-07-14
DAXINGANLING LINGOBERRY BOREAL BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the shortcomings of conventional techniques such as relatively low extraction rate and low extraction purity, and provide a preparation method for enriching and purifying agrimonin in Agrimony by high-speed countercurrent chromatography

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Using ethyl acetate-n-butanol-water and chloroform-methanol-isopropanol-water two-solvent system to prepare agridin with a purity higher than 98%: use a semi-preparative high-speed countercurrent chromatograph equipped with an NS-1007 pump, 20ml injection valve, polytetrafluoroethylene column, the volume of the column is 240ml, 8823A-UV ultraviolet detector Yokogawa 3057 portable recorder. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 800rpm, and pump the mobile phase into the column at a flow rate of 2.0ml / min. Detector UV spectra to receive target components. The preparation of Agrimidin is carried out in two steps: (1) Ethyl acetate-n-butanol-water with a volume ratio of 1:2:3 is miscible in a separatory funnel, shaken up and then separated into layers. Get the upper layer solution (upper phase) as the stationary phase, and the lower layer solution (lower phase) as the mobile phase. Dissolve 100 mg of ...

Embodiment 2

[0017] Agrimin with a purity higher than 98% was prepared using ethyl acetate-isobutanol-acetone-water and chloroform-methanol-water two-solvent system: using a semi-preparative high-speed countercurrent chromatograph equipped with a NS-1007 pump, 20ml into Sample valve, polytetrafluoroethylene column, the volume of the column is 240ml, 8823A-UV ultraviolet detector Yokogawa 3057 portable recorder. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 800rpm, and pump the mobile phase into the column at a flow rate of 2.0ml / min. Detector UV spectra to receive target components. The preparation of Agrimin is carried out in two steps: (1) Ethyl acetate-isobutanol-acetone-water with a volume ratio of 5:40:1:60 is miscible in a separatory funnel, shaken up and then separated into layers . Get the upper layer solution (upper phase) as the stationary phase, and the lower layer solution (lower phase) as the mobile phase. Diss...

Embodiment 3

[0019] Using n-butanol-water and dichloromethane-isopropanol-chloroform-methanol-water two-solvent system to prepare agridin with a purity higher than 98%: using a semi-preparative high-speed countercurrent chromatograph equipped with an NS-1007 pump, 20ml injection valve, polytetrafluoroethylene column, the volume of the column is 240ml, 8823A-UV ultraviolet detector Yokogawa 3057 portable recorder. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 800rpm, and pump the mobile phase into the column at a flow rate of 2.0ml / min. Detector UV spectra to receive target components. The preparation of agridin is carried out in two steps: (1) n-butanol-water with a volume ratio of 45:53 is miscible in a separatory funnel, shaken and then separated into layers. Get the upper layer solution (upper phase) as the stationary phase, and the lower layer solution (lower phase) as the mobile phase. Dissolve 150 mg of crude extract o...

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Abstract

The invention belongs to the filed of natural organic chemistry and relates to a method for purifying agrimonine, in particular to a method for gathering and purifying the agrimonine in agrimony by utilizing high-speed counter current chromatography. The method is characterized in that leaching liquor of natural plant agrimony is purified twice by utilizing the high-speed counter current chromatography, thus obtaining the agrimonine with the purity of 98 percent. The method is suitable for preparing the high-purity agrimonine by adopting various natural plants and extracts of the natural plants containing the agrimonine as the main materials. The method is suitable for separating and preparing the agrimonine by adopting a counter current chromatograph of various types, and the method for preparing the agrimonine by utilizing the high-speed counter current chromatography can carry out continuous, efficient and rapid liquid-liquid partition chromatographic separation and has the advantages of large separation amount, no sample loss, high recovery rate, mild separation environment, saving solvent and the like.

Description

Technical field: [0001] The invention belongs to the field of natural organic chemistry, and relates to a method for purifying agrimonin, in particular to a preparation method for enriching and purifying agrimonin in Agrimony by using a high-speed countercurrent chromatographic separation method. Background technique: [0002] Agrimonia: A general term for plants of the genus Agrimonia in the family Rosaceae, especially A. eupatoria. This species is a hardy perennial herb native to Europe and also cultivated in other warm regions. 30-100cm high, the whole plant has white long hairs, the rhizome is horizontal, cylindrical, and a conical upward curved white branch sprouts from the apex in late autumn. Stems erect. Odd-pinnate compound leaves alternate, leaflets vary in size, arranged at intervals, oval to obovate, stipules ovate. Racemes terminal or axillary, flowers small, yellow, calyx chrysanthemum with grooves and hairs on the outside, a circle of hook-shaped bristles o...

Claims

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Application Information

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IPC IPC(8): C07D519/00A61P15/00A61P7/04A61P1/00
Inventor 姚德坤姚德利闫峰姚航
Owner DAXINGANLING LINGOBERRY BOREAL BIOTECH CO LTD
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