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Method for extracting and separating stilbene glucoside from polygonum multiflorum

A stilbene glycoside, Polygonum multiflorum technology, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives and other directions, can solve the problem of large amount of extraction solvent water or ethanol, achieve less amount of extraction solvent and reduce extraction The amount of solvent and the effect of simple process

Inactive Publication Date: 2010-07-28
卢昶年 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method described in this invention is easier to operate and has higher extraction purity, but it also has the disadvantage of a large amount of extraction solvent water or ethanol

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1) Take Radix Polygoni Multiflori, crush it to 10 meshes, weigh 50kg, moisten and dissolve with 1 times the weight of the raw material and 20% ethanol solution, and place it for 1 hour after it is fully uniform; put it into a percolation tank, cover and soak for 30 hours, and then use the raw material 5 times the weight, 20% ethanol percolation extraction at room temperature, the percolation speed is 1BV / h, and the percolation time is 6h;

[0032] 2) Pass the extract through an ADS-7 macroporous resin column, elute with 3 times the resin weight and 60% ethanol at a flow rate of 1 BV / h, and collect the eluate;

[0033] 3) concentrating the eluent by reverse osmosis to 0.5 times the weight of the raw material;

[0034] 4) Add 0.3% acetic acid of the concentrated solution quality to the concentrated solution, leave it for 24 hours, the precipitated crystals are recrystallized under the same conditions, freeze-dried to obtain 2.52 kg of white needle-shaped stilbene glycosid...

Embodiment 2

[0036] 1) Take Polygonum multiflorum, crush it to 20 mesh, weigh 80kg, first use 0.75 times the weight of the raw material to moisten and dissolve, and place it for 2 hours after it is fully uniform; put it into a percolation tank, cover and soak for 40 hours, and then use 10 times the weight of the raw material Water percolation extraction at room temperature, the percolation rate is 0.8BV / h, and the percolation time is 10h;

[0037] 2) Pass the extract through an ADS-21 macroporous resin column, elute with 2.5 times the resin weight and 55% ethanol at a flow rate of 0.8 BV / h, and collect the eluate;

[0038] 3) concentrating the eluate by reverse osmosis to 0.8 times the weight of the raw material;

[0039] 4) Add 0.5% formic acid of concentrated solution quality to the concentrated solution, leave it for 30 hours, the crystals separated out are recrystallized under the same conditions, and freeze-dried to obtain 4.16 kg of white needle-like crystal stilbene glycosides, the ...

Embodiment 3

[0041] 1) Take Radix Polygoni Multiflori, crush it to 10 mesh, weigh 100kg, moisten and dissolve it with 1 times the weight of the raw material and 30% methanol solution, and place it for 1 hour after it is fully uniform; put it into a percolation tank, cover and soak for 30 hours, and then use the raw material 14 times the weight, 30% methanol percolation extraction at room temperature, the percolation rate is 0.8BV / h, and the percolation time is 5h;

[0042] 2) Pass the extract through an ADS-17 macroporous resin column, elute with 3 times the resin weight and 60% methanol at a flow rate of 0.8 BV / h, and collect the eluate;

[0043] 3) concentrating the eluate by reverse osmosis to 0.6 times the weight of the raw material;

[0044] 4) Add 0.4% formic acid in the concentrated solution to the concentrated solution, leave it for 32 hours, recrystallize the precipitated crystals under the same conditions, and freeze-dry to obtain 5.31 kg of white needle-shaped stilbene glycoside...

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PUM

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Abstract

The invention discloses a method for extracting and separating stilbene glucoside from polygonum multiflorum. The polygonum multiflorum is pulverized and extracted by water or low carbon ethanol percolation; and the extracted liquid is carried out macroporous resin column chromatography, reverse-osmosis concentration, crystallization, recrystallization and freezing for drying to obtain the stilbene glucoside. Compared with the prior art, the invention adopts normal temperature percolation extraction and can prevent the damage to the stilbene glucoside by carrying out extraction at high temperature in addition to have the advantages of less dosage of extracting solvent, few impurity, convenient operation, and the like; the following adopted reverse-osmosis concentration and freezing for drying both adopt low-temperature operation, and the damage to the stilbene glucoside is controlled to the lowest extent; furthermore, the organic acid is added into the concentrated liquid to carry out crystallization and recrystallization, which can change the PH value of a crystallized solution and is beneficial to crystallization, and can favorably protect the stilbene glucoside from being damaged. The purity of the product prepared by the method can reach more than 99 percent (detected by a high performance liquid chromatography (HPLC) method), and the yield of the product can reach more than 5.0 percent.

Description

technical field [0001] The invention relates to a method for extracting natural active ingredients in Chinese herbal medicines, in particular to a method for extracting and separating stilbene glycosides from Radix Polygoni Multiflori. Background technique [0002] Polygonum multiflorum, also known as Shouwu and Chishouwu, is the dry root tuber of Polygonum multiflorumthunb, a plant of the Polygonaceae family. Modern medicine shows that Polygonum multiflorum has multiple functions such as enhancing immune function, anti-oxidation, delaying brain aging, improving DNA repair function, prolonging life, lowering cholesterol, and improving fat metabolism. The main components of Radix Polygoni Multiflori are hydroxyanthraquinone compounds (mainly emodin, rheum, rhein and other glucosides, all of which are stilbene compounds), quinone compounds, stilbene glycoside compounds, amide compounds, color Protoketones, lecithin, trace elements calcium, iron, zinc, manganese, copper, etc. ...

Claims

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Application Information

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IPC IPC(8): C07H15/18C07H1/08
Inventor 卢昶年卢照凯
Owner 卢昶年
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