Separation and purification process of tetrahydroxy stilbeneglycoside

A tetrahydroxy stilbene, separation and purification technology, applied in organic chemistry, chemical instruments and methods, preparation of sugar derivatives, etc., can solve the problems of large sample loss, low recovery rate, unstable separation and purification, etc., to simplify separation Purification steps, overall process conditions are mild, soluble and stable

Inactive Publication Date: 2012-09-12
FOURTH MILITARY MEDICAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Tetrahydroxystilbene glycosides are polyphenolic glycosides. Their structural characteristics such as strong polarity, presence of sensitive groups (phenolic hydroxyl groups), easy formation of hydrogen bonds, and instability under extreme conditions make their separation and purification quite challenging. sex
Although this method can obtain pure TSG, in view of the limited availability of pure stilbene glycosides, it is not enough to systematically optimize the process conditions for crystallization
In addition, polyols often require repeated recrystallization to meet the purity requirements, which has long cycle times and low recovery rates, making them unsuitable for industrial production.
[0012] Lu Yunru et al. (Chinese inventi

Method used

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  • Separation and purification process of tetrahydroxy stilbeneglycoside
  • Separation and purification process of tetrahydroxy stilbeneglycoside
  • Separation and purification process of tetrahydroxy stilbeneglycoside

Examples

Experimental program
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Embodiment 1

[0035] Weigh 100 g (80 mesh) of Radix Polygoni Multiflori powder and put it in a beaker, add 200 mL of industrial ethanol, ultrasonically extract for 10 minutes, let stand, separate the supernatant, and spin off the solvent to obtain a brown extract. In the brown extract, add diethyl ether to soak, and filter to remove the ether layer after 0.5 h. The extracted extract after cold soaking in ether is fully dissolved by adding water, and the insoluble impurities are removed by filtration. The filtrate was extracted with ethyl acetate until the ester layer had no absorption point. The ester layer was collected and the solvent was removed to obtain a brown crude product. The crude product was adjusted to pH=9 with 1mol / L sodium hydroxide, and extracted with ethyl acetate until the ester layer had no absorption point. Leave the water layer. Cyclohexane was added to the water layer, and ethanol and water formed an azeotrope (the volume ratio of the three was 70%:7%:23%, and the b...

Embodiment 2

[0037]Weigh 500 g (80 mesh) of Radix Polygoni Multiflori powder and put it in a beaker, add industrial ethanol and ultrasonically extract for 10 minutes, let it stand, separate the supernatant, and spin off the solvent to obtain a brown extract. In the brown extract, add diethyl ether to soak, and filter to remove the ether layer after 0.5 h. Add water to fully dissolve the extracted extract after ether cold soaking, and filter to remove insoluble impurities. The filtrate was extracted with ethyl acetate until the ester layer had no absorption point. The ester layer was collected and the solvent was removed to obtain a brown crude product. The crude product was adjusted to pH=8.5 with 1mol / L sodium bicarbonate, and extracted with ethyl acetate until the ester layer had no absorption point. Leave the water layer. Cyclohexane was added to the water layer, ethanol and water formed an azeotrope, and the solvent was spun off to obtain crude TSG salt. The crude product was recry...

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Abstract

The invention discloses a separation and purification process for extracting tetrahydroxy stilbeneglycoside from roots and stems of Polygonum multiflorum. The process comprises the following steps of: firstly, extracting the Polygonum multiflorum by ethanol to obtain a leaching solution; removing an ethanol solvent to obtain a brown extract; adding ethyl ether into the brown extract to carry out cold soaking treatment and removing an ether layer; adding water into an extract obtained by the cold soaking treatment to dissolve; utilizing ethyl acetate to extract and collect an ester layer; removing a solvent to obtain a brown crude product; adding alkali liquid into the crude product to adjust a pH (Potential of Hydrogen) to 8-10; then utilizing the ethyl acetate to extract; adding cyclohexane and ethanol into an extracted water layer; carrying out rotary evaporation to remove the solvent to obtain a TSG (TetrahydroxyStilbene Glucoside) salt crude product; and acidifying and extracting by the ethyl acetate to obtain a pure product. According to the separation and purification process disclosed by the invention, various complicated column chromatographs are avoided and a synthesis process is greatly simplified; and whole process conditions are moderate, and a toxic and harmful solvent is not used, so that the separation and purification process is suitable for industrial production.

Description

technical field [0001] The invention relates to a separation and purification process for extracting stilbene glycoside monomers from the rhizomes of Polygonum multiflorum, belonging to the technical field of separation and extraction of natural products. Background technique [0002] Vascular dementia (VD) refers to a group of advanced neurocognitive dysfunctions based on brain tissue damage caused by ischemic, hemorrhagic, and acute and chronic ischemic-hypoxic cerebrovascular diseases. It is the second leading cause of dementia after Alzheimer's disease. Its clinical manifestations include memory impairment, cognitive impairment, personality changes, loss of orientation, abnormal behavior, and low daily social and living abilities. According to the epidemiological survey, VD accounts for about 20% of senile dementia in European and American countries, and about 60% in my country; the prevalence rate of VD in Japan reaches 1.1%-3.0%. With the acceleration of the aging pr...

Claims

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Application Information

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IPC IPC(8): C07H15/203C07H1/08
Inventor 何炜张旭王四旺张俊娜王宝龙张邦乐
Owner FOURTH MILITARY MEDICAL UNIVERSITY
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