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A method for preparing 3,6'-dierucanoyl sucrose ester from polygala

A technology of sinapinyl sucrose ester and sinapinyl sucrose, which is applied in the field of medicine, can solve the problems of being unable to meet the needs of scientific research and new drug development, high cost, and low yield, and achieve the goals of reducing production cost, improving work efficiency, and high yield Effect

Active Publication Date: 2015-09-16
洛阳泽达慧康医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, only 24.6 mg of 3,6'-dierucanoyl sucrose ester with a purity of 93% can be isolated from 500 g of Polygala medicinal material, and the yield is low (less than 1%) and the cost is high
According to research, the purity of the 3,6'-dierucanoyl sucrose ester reference substances currently available on the market is mostly around 90%, which cannot meet the needs of scientific research and new drug development

Method used

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  • A method for preparing 3,6'-dierucanoyl sucrose ester from polygala
  • A method for preparing 3,6'-dierucanoyl sucrose ester from polygala
  • A method for preparing 3,6'-dierucanoyl sucrose ester from polygala

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Experimental program
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Effect test

Embodiment 1

[0037] Take 2.00kg of the medicinal material Polygala (the content of 3,6'-dierucanoyl sucrose ester is 0.51%), put it into an extraction tank filled with 20L 60% ethanol solution, reflux extraction for 2 hours, extract twice, filter, and combine the extracts, Concentrate to dryness under reduced pressure at 50°C in the dark. Add water to disperse, centrifuge at 4000r / min for 30min, take the supernatant and add it to D101 macroporous resin. 3BV / h. After detection by high-performance liquid chromatography, the fractions containing 3,6’-dierucanoyl sucrose ester were combined, concentrated to dryness under reduced pressure below 50°C in the dark, and dissolved by adding ethanol-acetonitrile-water solution (12:3:85). After centrifugation at 4000r / min for 30min, the supernatant was taken, added to a medium-pressure preparative column (C18ME packing, 50μm, 100A), and eluted with ethanol-acetonitrile-water solution (12:3:85) at a rate of 40BV / h. After detection by high-performance...

Embodiment 2

[0039]Take 2.00kg of the medicinal material Polygala (the content of 3,6'-dierucanoyl sucrose ester is 0.51%), put it into an extraction tank filled with 20L 60% ethanol solution, reflux extraction for 2 hours, extract twice, filter, and combine the extracts, Concentrate to dryness under reduced pressure at 50°C in the dark. Add water to disperse, centrifuge at 4000r / min for 30min, take the supernatant and add it to D101 macroporous resin. 3BV / h. After detection by high-performance liquid chromatography, the fractions containing 3,6’-dierucanoyl sucrose ester were combined, concentrated to dryness under reduced pressure below 50°C in the dark, and dissolved by adding ethanol-acetonitrile-water solution (13.5:4.5:82). After centrifugation at 4000r / min for 30min, the supernatant was added to a medium-pressure preparative column (C18ME packing, 50μm, 100A), and eluted with ethanol-acetonitrile-water solution (13.5:4.5:82) at a rate of 40BV / h. After detection by high-performance...

Embodiment 3

[0041] Take 2.00kg of the medicinal material Polygala (the content of 3,6'-dierucanoyl sucrose ester is 0.51%), put it into an extraction tank filled with 20L 60% ethanol solution, reflux extraction for 2 hours, extract twice, filter, and combine the extracts, Concentrate to dryness under reduced pressure at 50°C in the dark. Add water to disperse, centrifuge at 4000r / min for 30min, take the supernatant and add it to D101 macroporous resin. 3BV / h. After detection by high-performance liquid chromatography, the fractions containing 3,6’-dierucanoyl sucrose ester were combined, concentrated to dryness under reduced pressure at 50°C in the dark, and dissolved by adding ethanol-acetonitrile-water (15:5:80). After centrifugation at 4000r / min for 30min, the supernatant was added to a medium-pressure preparative column (C18ME packing, 50μm, 100A), and eluted with ethanol-acetonitrile-water (15:5:80) at a rate of 40BV / h. After detection by high-performance liquid chromatography, the ...

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Abstract

The invention provides a method for preparing 3,6'-dimustard acyl sucrose ester from polygala tenuifolia. The method adopting the polygala tenuifolia medicine as the material comprises the following steps of: adding a proper amount of solvent, and extracting to obtain polygala tenuifolia extract liquor by adopting a heating reflux method, a percolation method or an ultrasonic method; enriching 3,6'-dimustard acyl sucrose ester by using macroporous adsorption resin, and purifying by using a medium-pressure chromatographic column to obtain the 3,6'-dimustard acyl sucrose ester with purity more than 98%. According to the method for preparing 3,6'-dimustard acyl sucrose ester from polygala tenuifolia disclosed by the invention is simple to operate and high in product purity; the adopted macroporous adsorption resin, and the inverted-phase medium-pressure chromatographic material can be repeatedly used; organic phases for eluting also can be repeatedly used after being recycled, so that the working efficiency is improved and the production cost is lowered, and therefore, the method can be suitable for expanding the industrial production.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a method for preparing high-purity 3,6'-dierucanoyl sucrose ester from polygala. Background technique [0002] 3,6'-Dierucanoyl sucrose (3,6'-disinapoylsucrose, DISS) is an acylated oligosaccharide, molecular formula: C 34 h 42 o 19 , Molecular weight: 754.23, light yellow amorphous powder. The molecular structural formula is as follows: [0003] [0004] 3,6'-Dierucanoyl sucrose ester has a clear antidepressant effect, can significantly improve the behavioral indicators of depression model mice, can enhance the function of the 5-HT system, and can protect damaged nerve cells. Rat HPA axis hormone levels can regulate, increase the expression of phosphorylated CREB in the hippocampus of depressed animals, and increase the mRNA and protein expression of CREB's downstream target gene BDNF. [0005] 3,6'-Dierucanoyl sucrose ester is mainly derived from polygala Polygala tenui...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H13/04C07H1/08
Inventor 栾连军施琦渊吴永江刘雪松雷后亮
Owner 洛阳泽达慧康医药科技有限公司