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Method for preparing high-purity hispidulin and herba lycopi flavone

A technology of high psyllium and zelan flavonoids is applied in the field of preparation of high-purity psyllium and zelan flavonoids, which can solve the problems of large solvent consumption, adsorption of samples, low distribution efficiency and the like, and achieves a large separation amount. , the separation environment is relaxed, the effect of saving solvent

Active Publication Date: 2011-06-15
SHANGHAI TAUTO BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the traditional liquid chromatography technology separates the preparation amount, 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; while HSCCC can guarantee a higher peak resolution, It has the advantages of simple operation, large separation volume, no sample loss, high separation efficiency, 100% theoretical recovery rate, good reproducibility and mild separation environment. It has been widely used in the preparation of chemical substances in the fields of biology, medicine, and environmental protection. separation and purification

Method used

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  • Method for preparing high-purity hispidulin and herba lycopi flavone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The trichloromethane-tetrachloromethane-ethanol-water system was selected to separate and purify the flavonoids of Lychee Grass on a semi-preparative countercurrent chromatograph. The suitable temperature for the experiment is 25°C. Firstly, the above-mentioned solvent components are distributed in a separatory funnel according to the volume ratio of 0.5:4:2:6, shaken and 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 100mg of Lychee Grass crude sample and dissolve it in a solution composed of 10ml upper phase and 10ml 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 ...

Embodiment 2

[0038] Tetrachloromethane-n-butanol-ethanol-water system was selected on a semi-preparative countercurrent chromatograph to separate and purify flavonoids from Lychee Grass. 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 of Lychee Grass crude 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 p...

Embodiment 3

[0040] The dichloromethane-chloroform-methanol-water system was selected to separate and purify the flavonoids of Lychee Grass 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 0.5:4:3:2, 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 150mg of Lychee Grass crude 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 i...

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Abstract

The invention relates to a preparation method for separating high-purity hispidulin and herba lycopi flavone from common sage herb by high-speed countercurrent chromatography. The preparation method comprises the following steps of: (1) preparing a proper solvent system and standing to laminate so as to obtain an upper phase and a lower phase; (2) selecting the upper phase as a stationary phase and the lower phase as a mobile phase, filling the fixed phase into a countercurrent chromatograph column, adjusting the rotating speed of a host to be 600 to 1,000 rpm, pumping the mobile phase into the column at the flow velocity of 0.5 to 5.0 ml / min, and performing sample introduction by a sample valve after the whole system establishes dynamic balance; and (3) receiving target components according to a detector ultraviolet spectra, concentrating and crystallizing to obtain the high-purity hispidulin and herba lycopi flavones. The method is applicable to various types of high-speed countercurrent chromatographs and preparation of calycosin with different content, and has the characteristics of large separation quantity, high recovery rate and simpleness and convenience of operation.

Description

technical field [0001] The invention belongs to the field of preparation of natural flavonoids, and in particular relates to a preparation method of high-purity high psyllium and eupatorium flavonoids. Background technique [0002] Litchigrass (Salvia plebeia R.Br.) is the aerial part of the Lamiaceae Salvia plant, also known as toad grass, snow primrose, holly and so on. Annual or biennial erect herbaceous plant, distributed in other regions except the northwest, mainly produced in Jiangsu, Zhejiang, Anhui and other provinces. Litchi grass crude extract to CCl 4 and D-GlaN induced acute liver injury in rats have protective effects, Oshima et al. found that high psyllogens, high psylloids and euphratica flavonoids in Litchi grass have a protective effect on CCl 4 And D-GlaN induces rat liver cytotoxicity to have protective effect (1mg / kg, p<0.001, the research such as Ferrandiz shows that high psyllium has protective effect to bromobenzene-induced mouse liver injury and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/30C07D311/40
Inventor 王维娜邓秋云
Owner SHANGHAI TAUTO BIOTECH CO LTD
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