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Method for preparing high-purity calycosin

A technology of high-purity multi-isoflavone, applied in the field of preparation of high-purity multi-isoflavone, can solve the problems of large solvent consumption, low distribution efficiency, sample adsorption, etc., and achieves the effects of large separation volume, solvent saving, and separation environment alleviation.

Active Publication Date: 2011-04-27
SHANGHAI TAUTO BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

When the traditional liquid chromatography technology is used for the separation of preparation volume, the distribution efficiency is low, the solvent consumption is large, and the solid support or carrier will cause problems such as adsorption, loss and denaturation of the sample

Method used

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  • Method for preparing high-purity calycosin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Select methyl acetate-n-propanol-ethanol-water system on a semi-preparative countercurrent chromatograph to separate and purify astragalus calycosin. The suitable temperature for the experiment is 20°C. Firstly, the above-mentioned solvent components are distributed and placed in a separatory funnel according to the volume ratio of 4:0.8:2:2, shaken and then allowed to stand for stratification. After equilibrating for a period of time, separate the upper and lower phases. A semi-preparative countercurrent chromatograph is used, equipped with a polytetrafluoroethylene column, a 20ml injection valve, a column volume of 300ml, a TBP-50A pump, a TBD-23 detector and an N2000 chromatographic workstation. Weigh 100 mg of Astragalus crude sample and dissolve it in a solution composed of 10 ml upper phase and 10 ml lower phase for use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 950rpm, and pump the mobile phase ...

Embodiment 2

[0035] Select ethyl acetate-n-butanol-ethanol-water system on a semi-preparative countercurrent chromatograph to separate and purify astragalus calycosin. The suitable temperature for the experiment is 30°C. Firstly, the above-mentioned solvent components are distributed and placed in a separatory funnel according to the volume ratio of 3:0.5:1:8, shaken and then allowed to stand for stratification. After equilibrating for a period of time, separate the upper and lower phases. A semi-preparative countercurrent chromatograph is used, equipped with a polytetrafluoroethylene column, a 20ml injection valve, a column volume of 300ml, a TBP-50A pump, a TBD-23 detector and an N2000 chromatographic workstation. Weigh 150mg crude astragalus sample and dissolve in 10ml upper phase and 10ml lower phase solution for later use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 650rpm, and pump the mobile phase into the column at ...

Embodiment 3

[0037]Select butyl acetate-n-propanol-ethanol-water system to separate and purify astragalus calycosin isoflavones on a semi-preparative countercurrent chromatograph. The suitable temperature for the experiment is 22°C. Firstly, the above-mentioned solvent components are distributed in a separatory funnel according to the volume ratio of 4:1:1:6, shaken and allowed to stand to separate into layers. After equilibrating for a period of time, separate the upper and lower phases. A semi-preparative countercurrent chromatograph is used, equipped with a polytetrafluoroethylene column, a 20ml injection valve, a column volume of 300ml, a TBP-50A pump, a TBD-23 detector and an N2000 chromatographic workstation. Weigh 150mg crude astragalus sample and dissolve in 10ml upper phase and 10ml lower phase solution for later use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 750rpm, and pump the mobile phase into the column at a...

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Abstract

The invention relates to a method for separating high-purity calycosin from a leguminous plant astragalus root by using high-speed countercurrent chromatography, comprising the following steps of: (1) preparing an appropriate solvent system, standing and delaminating to obtain a top phase and a bottom phase; (2) selecting the top phase as a fixed phase and the bottom phase as a mobile phase, firstly filling a countercurrent chromatograph column by using the fixed phase, regulating the rotating speed of a principal machine at 600-1000 rpm, pumping the mobile phase into the countercurrent chromatograph column at the flow rate of 0.5-4 ml / minute, and sampling through a sampling valve after the integral system establishes dynamic balance; and (3) receiving a target component according to an ultraviolet spectrum of a detector, and concentrating and crystallizing to obtain the calycosin. The preparation method is suitable for various types of high-speed countercurrent chromatographs and the preparation of various contents of the calycosin and has large separation amount, high recovery rate and easy and convenient operation.

Description

technical field [0001] The invention belongs to the field of isoflavone preparation, in particular to a preparation method of high-purity calycosin isoflavone. Background technique [0002] Astragalus membranaceus is the root of the perennial herbaceous plant Astragalus mongolica or Astragalus membranaceus. It is mainly used for lack of food and loose stools, depression of central Qi, chronic diarrhea of ​​the anus, blood in the stool and metrorrhagia, spontaneous perspiration due to surface deficiency, edema due to Qi deficiency, uterine prolapse, chronic nephritis, proteinuria, diabetes, and long-term non-healing of the mouth. Mongolian Astragalus membranaceus is the authentic Astragalus membranaceus recorded in the 2005 edition of the "Chinese Pharmacopoeia", and it is listed as the top grade in "Shen Nong's Materia Medica". The main ingredients are calycosin, actocoside, formononetin and formononetin, etc. [0003] The structural formula of calycosin is as follows: ...

Claims

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Application Information

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IPC IPC(8): C07D311/36C07D311/40
Inventor 王维娜邓秋云
Owner SHANGHAI TAUTO BIOTECH CO LTD
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