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A kind of preparation method of high-purity bergamot lactone and psoralen

A technology of bergamot lactone and psoralen, applied in the direction of organic chemistry and the like, can solve the problems of large solvent consumption, loss and denaturation, low distribution efficiency, etc., and achieve the effects of large separation amount, easy operation and solvent saving.

Active Publication Date: 2015-08-05
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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  • A kind of preparation method of high-purity bergamot lactone and psoralen
  • A kind of preparation method of high-purity bergamot lactone and psoralen

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Experimental program
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Effect test

Embodiment 1

[0034] The methyl acetate-n-propanol-ethanol-water system was selected to separate and purify bergamotide and psoralen on a semi-preparative countercurrent chromatograph. The suitable temperature for the experiment is 25°C. Firstly, the above-mentioned solvent components are distributed and placed in a separatory funnel according to the volume ratio of 4:0.8:2:6, 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 300mg crude fig 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 mobile phase into...

Embodiment 2

[0036] The ethyl acetate-n-butanol-ethanol-water system was selected to separate and purify bergamotide and psoralen on a semi-preparative countercurrent chromatograph. 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 fig sample and dissolve in 10ml upper phase and 10ml lower phase solution for 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

[0038]The butyl acetate-n-propanol-ethanol-water system was selected to separate and purify bergamotide and psoralen 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 fig sample and dissolve in 10ml upper phase and 10ml lower phase solution for 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 flow rate ...

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Abstract

The invention relates to a preparation method for separating high-purity bergapten and psoralen from ficus carica by using a high speed countercurrent chromatography method. The method comprises the following steps of: (1) preparing a proper solvent system, and standing still for layering to obtain an upper phase and a lower phase; (2) selecting the upper phase as a fixed phase and the lower phase as a flowing phase; filling a countercurrent chromatograph column with the fixed phase, and regulating the rotating speed of a host to be 600-1,000rpm; pumping the flowing phase into the column with a flowing speed of 0.5-5.0ml / min, and after dynamic balance of the whole system is established, introducing the sample through a sample introduction valve; and (3) receiving a target ingredient according to an ultraviolet spectrum of a detector, and then concentrating and crystallizing to obtain the finished product. The method is suitable for the preparation of various types of high speed countercurrent chromatographs as well as bergapten and psoralen of various contents and has the characteristics of large separation quantity, high recovery rate and simpleness and convenience for operation.

Description

technical field [0001] The invention belongs to the field of preparation of coumarin components, in particular to a preparation method of high-purity bergamot lactone and psoralen. Background technique [0002] Fig is a plant of the genus Ficus Carica L of the family Moraceae. The fruit of fig contains a variety of amino acids needed by the human body, and is rich in vitamins such as VA and VC. It not only tastes sweet, but also has great medicinal value. . In traditional Chinese medicine, figs are mainly used for "strengthening the stomach and clearing the intestines, reducing swelling and detoxification" and treating enteritis, dysentery, and hemorrhoids. In addition to treating hemorrhoids, swollen poison, and heartache, fig leaves also have certain antihypertensive and anticancer effects. Fig leaf extract has strong antibacterial activity and can be used in food as a natural preservative. Psoralen and bergapton are the main antibacterial components in fig leaf extract...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/04
Inventor 王维娜邓秋云
Owner SHANGHAI TAUTO BIOTECH CO LTD
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