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Method for purifying stilbene glucoside in Lysimachia clethroide duby

A stilbene glycoside and loosestrife technology, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve the problems of poor stability, difficult synthesis, complex structure of stilbene glycosides, etc.

Inactive Publication Date: 2012-10-10
FOURTH MILITARY MEDICAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Stilbene glycosides have complex structures, poor stability, and are difficult to synthesize. At present, they are all extracted and separated from Polygonum multiflorum.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Take 1 kg of pearl vegetable medicinal material, crush it into coarse powder, moisten it with 2000ml 60% ethanol; put it into a percolator; use 10000ml 60% ethanol for percolation, collect the percolation liquid; recover ethanol under reduced pressure, concentrate to 1200ml, and use 2400ml Ether extraction, a total of 3 extractions, to remove fat-soluble impurities; take the water layer, add 4000ml deionized water to dilute, centrifuge (3000 rpm) for 10 minutes, and the supernatant is passed through D-101 at a flow rate of 1L / (kg h). Pore ​​adsorption resin (column diameter-column height=1:10, the weight of the resin is 2 times the weight of the medicinal material), use deionized water 3 times the volume of the resin to remove impurities at a flow rate of 1L / (kg h), discard, and then Use 30% ethanol that is 5 times the volume of the resin to remove impurities at a flow rate of 0.8L / (kg h), and finally use 40% ethanol that is 6 times the volume of the resin to desorb at a...

Embodiment 2

[0014] Take 5kg of loosestrife medicinal material, crush it into coarse powder, wet it with 10L 70% ethanol; put it into a percolator; use 70L 70% ethanol for percolation, collect the percolation liquid; recover ethanol under reduced pressure, concentrate to 5L, and use 10L Ether extraction, a total of 3 extractions, to remove fat-soluble impurities; take the water layer, add 10L deionized water to dilute, centrifuge (3000 rpm) for 10 minutes, and supernatant flow through D-101 at a flow rate of 1L / (kg h). Pore ​​adsorption resin (column diameter-column height=1:10, the weight of the resin is 2 times the weight of the medicinal material), use deionized water 3 times the volume of the resin to remove impurities at a flow rate of 1L / (kg h), discard, and then Use 30% ethanol that is 4 times the volume of the resin to remove impurities at a flow rate of 0.8 L / (kg h), and finally use 40% ethanol that is 5 times the volume of the resin to desorb at a flow rate of 0.8 L / (kg h), and co...

Embodiment 3

[0016] Take 10kg of pearl vegetable medicinal material, crush it into coarse powder, moisten it with 15L 60% ethanol; put it into a percolator; use 100L 60% ethanol for percolation, collect the percolation liquid; recover ethanol under reduced pressure, concentrate to 8L, and use 2000ml Ether extraction, a total of 3 extractions, to remove fat-soluble impurities; take the water layer, add 30L deionized water to dilute, centrifuge (3000 rpm) for 10 minutes, and the supernatant is passed through D-101 at a flow rate of 1.2L / (kg h) Macroporous adsorption resin (column diameter-column height=1:8, the weight of the resin is 2 times the weight of the medicinal material), deionized water twice the volume of the resin is used to remove impurities at a flow rate of 1L / (kg h), discarded, Then use 30% ethanol that is 4 times the volume of the resin to remove impurities at a flow rate of 1 L / (kg h), and finally use 40% ethanol that is 6 times the volume of the resin to desorb with a flow r...

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PUM

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Abstract

The invention relates to a method for purifying stilbene glucoside in Lysimachia clethroide duby, which belongs to the extraction and separation technical fields of traditional Chinese medicine effective components. The preparation method comprises the following steps: coarse powder of Lysimachia clethroide duby is taken, extracted by using 40-80% ethanol, pressure reduction and concentration are carried out, and the coarse powder is extracted by using ethyl ether or petroleum ether, an aqueous solution is placed on a macroporous adsorbent resin column and preliminarily purifyed to obtain the crude product of stilbene glucoside; the crude product is loaded on a Sephadex column and separated by a LH-20 column, eluted by using chloroform and methanol with ratio of 1:1, and monitored by high performance liquid chromatography until no stilbene glucoside is existed in an eluate, pressure reduction and concentration are carried out, the coarse product is frozen and dried to obtain stilbene glucoside. The method of the invention has the advantages of high purity extraction, stable process, less loss of effective components and the like.

Description

technical field [0001] The invention belongs to the technical field of extraction and separation of effective components in traditional Chinese medicines, and in particular relates to a method for extracting and separating stilbene glycosides from pearls. Background technique [0002] 2,3,5,4'-Tetrahydroxystilbene-2-O-β-D-glucoside (referred to as stilbene glycoside), is a white amorphous powder, easily soluble in water, methanol, ethanol, and has important Medicinal value: It can significantly improve the learning and memory impairment of animal models of brain injury, and has therapeutic effects on neurodegenerative diseases such as senile dementia [Zhang Lan, Xing Ying, Zhao Ling, et al. Learning and memory of APP transgenic mice with different time courses Change and the intervention effect of Shenwu Capsules and stilbene glycosides. Chinese Behavioral Medicine Science, 2006, 15(3): 193-196]; it can scavenge free radicals, reduce the level of lipid peroxidation in the bo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/203C07H1/08
Inventor 曹蔚王四旺谢艳华杨倩孙纪元缪珊
Owner FOURTH MILITARY MEDICAL UNIVERSITY
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