Separation and purification process of 2, 3, 5, 4'-tetrahydroxystilbene-2-O-beta-D-glucoside

A technology of tetrahydroxystilbene and stilbene glycosides, which is applied in the field of separation and purification of stilbene glycosides (stilbene glycosides), can solve the problems of large solvent consumption, high instrument cost, and restricting development, so as to improve product purity, Good repeatability and wide applicability

Inactive Publication Date: 2014-01-22
TIANJIN UNIV OF TRADITIONAL CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This patented method allows for efficient isolation or purification of specific types of compounds called stiollenegalosylglycerols (SGL). By doing this it simplifies the way we work on these molecules by allowing them to pass through easily without being affected during processing steps like extraction. It also provides technical benefits such as ease of operation, environmental friendliness, lower costs compared to other methods used for producing pure S GL products.

Problems solved by technology

This patented technical solution involves separating polypegrana cuspina (Pcma) from plants called Lupinus multicillis variegatus (LMS). However, current techniques require expensive equipment and long processing time due to slow filtration processes. Therefore, new ways to efficiently isolate pure polysaphenoic acid compounds without these drawbacks would improve their effectiveness on various applications including prevention of diseases caused by harmful metabolites found within cells.

Method used

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  • Separation and purification process of 2, 3, 5, 4'-tetrahydroxystilbene-2-O-beta-D-glucoside
  • Separation and purification process of 2, 3, 5, 4'-tetrahydroxystilbene-2-O-beta-D-glucoside
  • Separation and purification process of 2, 3, 5, 4'-tetrahydroxystilbene-2-O-beta-D-glucoside

Examples

Experimental program
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Effect test

Embodiment 1

[0042] Use the extract of stilbene glycosides (50% purity of stilbene glycosides) to separate and purify stilbene glycosides, the specific steps are as follows:

[0043] (1) Weigh 110g of 50% stilbene glycoside extract, put it in a beaker, add 150ml of 95% (v / v) ethanol to fully mix and dissolve it, add 150g of silica gel (200-300 mesh) to mix the sample, and put it in Grind in a fume hood and allow the solvent to evaporate naturally to become loose;

[0044] (2) Mix 5000ml of ethyl acetate and 1000g of silica gel (100-200 mesh), stir to remove air bubbles, slowly pour into the glass column after soaking completely, and then continue to add ethyl acetate to remove the Wash the silica gel to make the silica gel on the surface of the glass column smooth;

[0045] (3) Slowly add the sample treated in step (1) on the prepared glass column, elute with ethyl acetate, 1 fraction per 600ml, collect 20 fractions in total, and track and detect them by TLC , combined 4-19, blue fluores...

Embodiment 2

[0048] Use the extract of stilbene glycosides (80%) to separate and purify stilbene glycosides, the specific steps are as follows:

[0049] Weigh about 70g of the stilbene glycoside sample (80% stilbene glycoside extract), put it in a beaker, heat and dissolve it with about 3 times the amount (210ml) of pure water I, and place it in a -10±1°C Freeze until it crystallizes under certain conditions and take it out. After melting at room temperature, transfer it to a suction filtration device for suction filtration, and wash it with 5 times the amount (350ml) of pure water II in small amounts. It can be seen that the filter residue is off-white crystals. Transfer the filter residue Dry in a vacuum drying oven under reduced pressure to obtain 41.59g of pure stilbene glycosides. After HPLC detection, the purity of stilbene glycosides is 96.50% after being treated with low-temperature water media. The results are shown in Figure 12 .

Embodiment 3

[0051] Separation and purification of stilbene glycosides with the extract of stilbene glycosides (50%), the specific steps are as follows:

[0052] (1) Weigh 100g of 50% stilbene glycoside extract, put it in a beaker, add 120ml of 95% ethanol to mix and dissolve it, add 200g of silica gel (200-300 mesh) to mix the sample, grind it in a fume hood and make it The solvent evaporates naturally and becomes loose;

[0053] (2) Mix 5000ml of ethyl acetate and 1000g of silica gel (100-200 mesh), stir to remove air bubbles, slowly pour into the glass column after soaking completely, and then continue to add ethyl acetate to remove the Wash the silica gel to make the silica gel on the surface of the glass column smooth;

[0054] (3) Slowly add the sample treated in step (1) on the prepared glass column, elute with ethyl acetate, 1 fraction per 600ml, collect 20 fractions in total, and track and detect them by TLC , combined 4-19, blue fluorescence can be observed at 365nm, combined t...

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Abstract

The invention provides a separation and purification process of 2, 3, 5, 4'-tetrahydroxystilbene-2-O-beta-D-glucoside (short for stilbene glucoside). The separation and purification process comprises the steps of weighting a stilbene glucoside extractive, stirring a sample by using silica gel until the sample is loosened, eluting the loosened sample on a glass column by using an eluent, tracking and checking through a thin layer chromatography (TLC), merging a stilbene glucoside contained component, recovering a solvent, and drying to obtain the stilbene glucoside extractive; adding pure water, heating to dissolve the stilbene glucoside extractive, then, freezing and crystallizing the solution, carrying out suction filtration after the frozen and crystallized solution is molten, and washing the solution with the pure water to obtain a white crystal; transferring filter residues to a vacuum drying oven for drying to obtain a pure product of stilbene glucoside. The process is simple and feasible in operation, capable of improving the product purity, and capable of quickly separating and purifying a large amount of stilbene glucoside. The process is simple and convenient to operate, low in cost, stable in yield, capable of obtaining high-purity stilbene glucoside after re-crystallization treatment while keeping low cost and high yield, and suitable for meeting the requirements for large-scale industrial production.

Description

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Claims

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Application Information

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Owner TIANJIN UNIV OF TRADITIONAL CHINESE MEDICINE
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