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
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[0029] Example 1: Weigh 49 kg of Polygonum multiflorum powder and place them in an extraction tank, and add 490 kg of medical alcohol to the extraction tank for three times soaking for 24 hours each time. The extracts after three soaking are combined, concentrated and centrifuged to obtain a clear Liquid A. After adding 98 g of gelatin to the clear solution A, adjust the pH to neutral with sodium hydroxide, let it stand for 30 minutes, and centrifuge to obtain clear solution B. Add 5 L of saturated copper chloride solution to clear liquid 2, stir and centrifuge to obtain clear liquid C. The clear liquid C was extracted with ether, and extracted 3 times at a volume ratio of 1:1. After combining the ether layers, the solvent was evaporated to obtain 900 g of crude TSG. The crude TSG product was recrystallized with water, and finally 850 g of pure TSG product was obtained, and its purity was 99.23% by high performance liquid chromatography.
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[0030] Example 2: Weigh 100 kg of Polygonum multiflorum powder and place it in an extraction tank, and add 1000 kg of medical alcohol to the extraction tank for three times soaking for 24 h each time. The extracts after the three soaking are combined, concentrated and centrifuged to obtain a clear solution. Liquid A. After adding 261g 101 clarifier to the clear liquid A, adjust the pH to neutral with potassium hydroxide, let it stand for 30 minutes, and centrifuge to obtain clear liquid B. Then add 10L of saturated copper acetate solution to the clear solution B, stir and centrifuge to obtain clear solution C. The clear liquid C was extracted with methyl formate, and extracted 3 times at a volume ratio of 1:1. After the methyl formate layers were combined, the solvent was removed to obtain 1850 g of crude TSG. The crude TSG product was recrystallized with ethanol, and finally 1700 g of pure TSG product was obtained. The purity of the product was 99.11% by high performance liqu...
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[0031] Example 3: Weigh 200 kg of Polygonum multiflorum powder and place them in an extraction tank. Add 2000 kg of 85% alcohol to the extraction tank for three times and soak for 24 hours each time. The extracts after three times of soaking are combined, concentrated, and centrifuged to obtain Clear liquid A. After adding 500 g of ZTC natural clarifying agent to the clear liquid A, adjust the solution to neutral with sodium carbonate, let it stand for 30 minutes, and centrifuge to obtain clear liquid 2. Add 2 L of saturated lead nitrate solution to clear solution B, stir and centrifuge to obtain clear solution C. The clear liquid C was extracted with dichloromethane, and extracted 3 times at a volume ratio of 1:1, the dichloromethane layers were combined, and the solvent was evaporated to obtain 4 kg of crude TSG. The crude TSG was recrystallized with acetone, and the final TSG pure product was 3.5 kg. The purity was 99.27% by high performance liquid chromatography.
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