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Process method for extracting and purifying tetrahydroxyl diphenylethylene glycoside from polygonum multiflorum

The technology of a tetrahydroxystilbene and a process method is applied in the field of biomedicine, can solve problems such as a low-cost separation and purification method, and achieves the effects of remarkable purification effect, high yield and mild process conditions

Inactive Publication Date: 2014-04-09
FOURTH MILITARY MEDICAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Obviously, there is no separation and purification method that is easy to operate, low in cost, and capable of large-scale industrial production.

Method used

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  • Process method for extracting and purifying tetrahydroxyl diphenylethylene glycoside from polygonum multiflorum

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1: Weigh 49 kg of Polygonum multiflorum powder and place it in an extraction tank, add 490 kg of medical alcohol into the extraction tank for soaking in three times, soak for 24 h each time, combine the extracts after three soaks, concentrate, centrifuge, and obtain clear Liquid A. After adding 98 g of gelatin to the supernatant A, adjust the pH to neutral with sodium hydroxide, let it stand for 30 minutes, and centrifuge to obtain the supernatant B. Add 5 L of saturated copper chloride solution to clear solution 2, stir and centrifuge to obtain clear solution C. The clear liquid C was extracted with diethyl ether, and extracted three times at a volume ratio of 1:1. After combining the diethyl ether layers, the solvent was evaporated to dryness to obtain 900 g of crude TSG. The crude product of TSG was recrystallized with water to finally obtain 850 g of pure product of TSG, and its purity was 99.23% as detected by high performance liquid chromatography.

Embodiment 2

[0030] Example 2: Weigh 100 kg of Polygonum multiflorum powder and place it in an extraction tank, add 1000 kg of medical alcohol into the extraction tank for soaking in three times, soak for 24 h each time, combine the extracts after three soaks, concentrate, centrifuge, and obtain clear Liquid A. After adding 261g of 101 clarifier to the clear liquid A, adjust the pH to neutral with potassium hydroxide, let it stand for 30min, and centrifuge to obtain the clear liquid B. Then add 10 L of saturated copper acetate solution to the supernatant solution B, centrifuge after stirring to obtain supernatant solution C. The clear liquid C was extracted with methyl formate, extracted three times according to the volume ratio of 1:1, after combining the methyl formate layers, the solvent was removed to obtain 1850 g of crude TSG. The crude product of TSG was recrystallized from ethanol to finally obtain 1700 g of pure product of TSG, and its purity was 99.11% as detected by high perfor...

Embodiment 3

[0031] Example 3: Weigh 200 kg of Polygonum multiflorum powder and place it in an extraction tank, add 2000 kg of 85% alcohol in three times to soak in the extraction tank, soak for 24 hours each time, combine the extracts after three soaks, concentrate, and centrifuge to obtain Serum A. After adding 500 g of ZTC natural clarifier to clear solution A, adjust the solution to neutral with sodium carbonate, let it stand for 30 minutes, and centrifuge to obtain clear solution 2. Add 2 L of saturated lead nitrate solution to supernatant B, stir and centrifuge to obtain supernatant C. The clear liquid C was extracted with dichloromethane three times at a volume ratio of 1:1, the dichloromethane layers were combined, and the solvent was evaporated to dryness to obtain 4 kg of crude TSG. The crude product of TSG was recrystallized with acetone to finally obtain 3.5 kg of pure product of TSG, which was detected by high performance liquid chromatography with a purity of 99.27%.

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Abstract

The invention discloses a process method for extracting and purifying tetrahydroxyl diphenylethylene glycoside from polygonum multiflorum. The process method comprises the following steps: (1) leaching polygonum multiflorum through alcohol to obtain clear liquid A; (2) adding a clarifying agent in the clear liquid A, adding an organic or inorganic alkali to regulate the solution to be neutral, and centrifuging to obtain clear liquid B; (3) adding a saturated metal ion precipitating agent in the clear liquid B; (4) extracting clear liquid C through an organic solvent, removing the organic solvent by distillation to obtain a crude product of tetrahydroxyl diphenylethylene glycoside, and recrystallizing to obtain a pure product of tetrahydroxyl diphenylethylene glycoside with purity larger than 99%. The process method disclosed by the invention is used for avoiding various complicated column chromatography processes and is high in yield and simple in process; the whole process is mild in conditions, environment-friendly and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a process method for extracting and purifying tetrahydroxystilbene glycosides from Polygonum multiflorum, in particular to a pilot-scale process method, which belongs to the field of biomedicine. Background technique [0002] Tetrahydroxystilbene glucoside (tetrahydroxystilbene glucoside, TSG), the chemical name is 2, 3, 5, 4'-tetrahydroxystilbene-2-O-β-D-glucoside, the structure is as follows, it is medicinal A bioactive component in the plant Polygonum multiflorum. [0003] [0004] Modern studies have found that TSG has the following pharmacological effects: ① TSG can obviously protect nerve cells and resist β-amyloid H 2 o 2 The resulting decrease in cell survival rate and increase in LDH leakage rate has obvious brain protection effects on the ischemia-reperfusion model, and can improve the learning, memory and cognitive functions of animals; ② TSG can remove excessive oxygen free radicals in the body and has Signifi...

Claims

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Application Information

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IPC IPC(8): C07H15/203C07H1/08
Inventor 何炜兰婷张俊娜王宝龙张邦乐
Owner FOURTH MILITARY MEDICAL UNIVERSITY
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