Separation and purification process of tetrahydroxy stilbeneglycoside

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...

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 invention patent ZL98120290.X) disclosed a method for extracting and separating TSG from Polygonum multiflorum. This method cuts the chromatographic column used for separation and purification destructively, and then samples and separates them. The process is cumbersome. High cost, only suitable for the preparation of micro samples in the laboratory

[0013] The above-mentioned documents or patent methods all involve various column chromatography separation methods. As we all know, the operation of column chromatography is cumbersome. On the one hand, the sample loss is relatively large, resulting in a low yield. On the other hand, the use of a large number of elution solvents increases the cost. Not suitable for large-scale industrial production

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