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Method for preparing stibene glucoside from fleece-flower root

A technology of stilbene glycosides and Polygonum multiflorum, which is applied in the field of natural medicinal chemistry, can solve the problems of complex stilbene glycosides methods and unsuitability for industrial production, and achieve the effect of high product yield and simple operation

Inactive Publication Date: 2013-08-14
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As mentioned above, the existing method for preparing stilbene glycosides is relatively complicated and is not suitable for industrialized production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Take 20kg of fresh Radix Polygoni Multiflori, clean it, chop it into a colloid mill to make pulp, and add appropriate amount of water to get 35kg of slurry, add 70L of 95% edible alcohol, stir for 2 hours, centrifuge, and add hollow cellulose sodium with a molecular weight cut-off of 800 to the centrifuge. Membrane filtration, add an appropriate amount of 70% ethanol for dialysis, collect the permeate, and then recover ethanol under reduced pressure. After the concentrated solution is cooled to room temperature, add 2 times the volume of ethyl acetate for full extraction, collect the ethyl acetate layer, and pass through 160 mesh Add 1 / 7 volume of petroleum ether and stir thoroughly, refrigerate and crystallize for 36 hours, filter out the crystals, dissolve in methanol, add an appropriate amount of ether to refrigerate and crystallize twice, the crystallized stilbene glycosides 71g, Through high-phase liquid phase detection, the content is 95.3%.

Embodiment 2

[0017] Take 20kg of fresh Polygonum multiflorum, clean it, chop it into a colloid mill, and add appropriate amount of water to get 35kg of slurry, add 70L of 95% edible alcohol, stir for 3 hours, centrifuge, and add hollow cellulose sodium with a molecular weight cut-off of 500 to the centrifuge. Membrane filtration, add an appropriate amount of 60% ethanol for dialysis, collect the permeate, and then recover ethanol under reduced pressure. After the concentrated solution is cooled to room temperature, add 2 times the volume of ethyl acetate for full extraction, collect the ethyl acetate layer, pass through 200 mesh Add 1 / 5 of the volume of petroleum ether and stir thoroughly, refrigerate and crystallize for 24 hours, filter out the crystals, dissolve in methanol, add an appropriate amount of ether to refrigerate and crystallize twice, and crystallize stilbene glycosides 56g, Through high-phase liquid phase detection, the content is 97.8%.

Embodiment 3

[0019] Take 20kg of fresh Radix Polygoni Multiflori, clean it, chop it into a colloid mill to make pulp, and add appropriate amount of water to get 35kg of slurry, add 70L of 95% edible alcohol, stir for 3 hours, centrifuge, and add hollow cellulose sodium with a molecular weight cut-off of 700 to the centrifuge Membrane filtration, add an appropriate amount of 50% ethanol for dialysis, collect the permeate, and then recover ethanol under reduced pressure. After the concentrated solution is cooled to room temperature, add 2 times the volume of ethyl acetate for full extraction, collect the ethyl acetate layer, and pass through 120 mesh Add 1 / 5 volume of petroleum ether and stir thoroughly, refrigerate and crystallize for 24 hours, filter out the crystals, dissolve in methanol, add an appropriate amount of ether to refrigerate and crystallize twice, the crystallized stilbene glycosides 63g, Through high-phase liquid phase detection, the content is 99.8%.

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PUM

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Abstract

The invention discloses a method for preparing stibene glucoside from fleece-flower root. The method comprises the following steps: (1) cleaning fresh fleece-flower root, pulverizing, pulping in a colloid mill, adding 2 times by volume of 95% edible alcohol to the pulp, sufficiently stirring, centrifuging, filtering the centrifugate through a nanofiltration membrane, collecting the permeation solution, recovering the ethanol under reduced pressure, adding ethyl acetate into the concentrated solution to carry out extraction, collecting the ethyl acetate layer, passing through an aluminum oxide short column, collecting the column solution, adding petroleum ether, and refrigerating to crystallize; and (2) filtering out the crystals, dissolving in methanol, adding a right amount of aether, refrigerating to crystallize 2-3 times, and drying the crystals. The method has the advantages of simple and manageable technique and high product yield, and can easily implement industrial production.

Description

technical field [0001] The invention belongs to the field of natural medicinal chemistry, in particular to a method for preparing stilbene glycosides from Radix Polygoni Multiflori. Background technique [0002] Polygonum multiflorum contains various medicinal ingredients such as stilbene compounds, anthraquinone compounds, polymerized proanthocyanidins, lecithin, amino acids, and trace elements. Stilbene glycosides are a class of water-soluble components with significant pharmacological activity, and their representative components are 2,3,5,4'-tetrahydroxystilbene-2-O-β-D-glucoside, referred to as two Styrene glycoside, molecular formula C20H22O9, molecular weight 406.38, easily soluble in methanol, ethanol, acetone, hot water, soluble in ethyl acetate, slightly soluble in cold water, hardly soluble in lipophilic solvents such as ether and chloroform. It has various health care functions such as delaying aging, preventing and fighting cancer, protecting the liver and brai...

Claims

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Application Information

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IPC IPC(8): C07H15/18C07H1/08
Inventor 刘东锋杨成东
Owner NANJING ZELANG MEDICAL TECH
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