Method for preparaing trans-resveratrol by hydrolyzing trans-polydatin
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A technology of resveratrol glycosides and resveratrol, which is applied in the field of preparation of trans-resveratrol by hydrolysis of trans-resveratrol glycosides, which can solve the problems of long time and low conversion rate of trans-resveratrol glycosides problem, to achieve the effect of low production cost, short hydrolysis time and improved extraction rate
Inactive Publication Date: 2011-09-07
ANHUI AGRICULTURAL UNIVERSITY
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[0007] In order to solve the problem that the enzymatic treatment takes a long time and the conversion rate of trans-resveratrol glycosides by simple acid hydrolysis is very low, the present invention provides a trans-resveratrol glycoside with high conversion rate and short hydrolysis time. Method for preparing trans-resveratrol by glycoside hydrolysis
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Embodiment 1
[0035] raw material:
[0036] Raw material A: trans-resveratrol glycosides (in milligrams or grams, with a purity of 90%),
[0037] Raw material C: pure methanol (in milliliters or liters),
[0038] Raw material D: hydrochloric acid (12%) (in milliliters or liters);
[0039] The optimum formula of the hydrolysis conversion system is A: C: D=4: 2: 2;
[0040] Preparation of hydrolysis conversion system:
[0041] Firstly weigh raw material A and dissolve it in raw material C solution, after fully dissolved, add raw material D solution.
[0042] Reaction conditions: put the hydrolysis conversion system at 55-65°C for 3h or 75°C for 1h; get the hydrolysis system;
[0043] After completion of the reaction, the hydrolysis system was purified by thin-layer chromatography on a silica gel plate, and the developing solvent used for the purification of thin-layer chromatography was: toluene: ethyl acetate: formic acid=5: 4: 1, and was mixed with The scrapings were obtained by scrapi...
Embodiment 2
[0057] raw material:
[0058] Raw material B: Polygonum cuspidatum dry powder (take 24 mesh, the unit is gram)
[0059] Raw material C: pure methanol (in milliliters or liters)
[0060] Raw material D: hydrochloric acid (12%) (in milliliters or liters);
[0061] The optimal formulation of the hydrolysis conversion system is B:C:D=1:10:10;
[0062] According to the above formula, dissolve the 20-mesh Polygonum cuspidatum dry powder in methanol, after fully dissolving, add 12% hydrochloric acid solution; at a temperature of 55-75°C, perform a hydrolysis reaction for 1-3 hours to obtain a hydrolysis system;
[0063] After the completion of the reaction, the hydrolysis system was purified by thin-layer chromatography on a silica gel plate, and the developing solvent used for the purification of thin-layer chromatography was: toluene: ethyl acetate: formic acid=5: 4: 1, and mixed with resveratrol under a 365nm ultraviolet lamp. Scrapes obtained by scraping off spots with the sam...
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Abstract
The invention relates to a method for preparing trans-resveratrol by hydrolyzing trans-polydatin, solving the problems that the prior enzyme process needs longer treatment time and has a very low convThe invention relates to a method for preparing trans-resveratrol by hydrolyzing trans-polydatin, solving the problems that the prior enzyme process needs longer treatment time and has a very low conversion rate by the simple acid hydrolysis of the trans-polydatin. The hydrolysis conversion system comprises the ingredients of trans-polydatin with the purity of 90 percent, methanol and hydrochloricersion rate by the simple acid hydrolysis of the trans-polydatin. The hydrolysis conversion system comprises the ingredients of trans-polydatin with the purity of 90 percent, methanol and hydrochloric acid solution with the purity of 12 percent which are in a ratio of 4 to 2 to 2; the trans-polydatin with the purity of 90 percent is fully dissolved into the methanol, and the hydrochloric acid soluacid solution with the purity of 12 percent which are in a ratio of 4 to 2 to 2; the trans-polydatin with the purity of 90 percent is fully dissolved into the methanol, and the hydrochloric acid solution with the purity of 12 percent is added to carry out a hydrolysis reaction for 1 hour to 3 hours at a temperature of 55 DEG C to 75 DEG C; a scraped matter is obtained by the hydrolysis system afttion with the purity of 12 percent is added to carry out a hydrolysis reaction for 1 hour to 3 hours at a temperature of 55 DEG C to 75 DEG C; a scraped matter is obtained by the hydrolysis system after the thin layer chromatography of a silica gel plate, dissolved in 3ml of methanol, ultrasonically cleaned, shaken and separated, and supernatant fluid is frozen to obtain the white powdered trans-rer the thin layer chromatography of a silica gel plate, dissolved in 3ml of methanol, ultrasonically cleaned, shaken and separated, and supernatant fluid is frozen to obtain the white powdered trans-resveratrol. Compared with the prior art, the method has high conversion rate of 45 percent, short hydrolysis time of 1 hour to 3 hours and simple operation and can recycle the methanol, thereby havingesveratrol. Compared with the prior art, the method has high conversion rate of 45 percent, short hydrolysis time of 1 hour to 3 hours and simple operation and can recycle the methanol, thereby havinglow production cost and being easy to realize industrialized production. low production cost and being easy to realize industrialized production.
Description
technical field [0001] The invention relates to a method for preparing trans-resveratrol by hydrolyzing trans-resveratrol glycosides. Background technique [0002] Resveratrol and its derivatives have a variety of pharmacological effects, and can be used for anticancer, antihypertensive and cardiovascular diseases, and have high value in clinical application. It mainly exists in 72 species of plants belonging to 12 families and 31 genera, including grapes, knotweed, peanuts, mulberries, pine trees, maima vines, and Korean pagoda tree. [0003] Polygonum cuspidum (polygonum cuspidtum Sieb. et Zucc.) is a perennial herbaceous plant belonging to the genus Polygonum. The dried rhizomes of Polygonum cuspidatum mainly contain anthraquinones, stilbenes, water-soluble polysaccharides and tannins. Resveratrol glycosides and resveratrol are the main stilbenes, of which resveratrol glycosides content is much higher than that of resveratrol, Wang Lei [1] The results of determination ...
Claims
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