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Method for preparing high-purity punicalagin crystal powder

A technology of punicalagin and crystalline powder, which is applied in the field of preparation of high-purity punicalagin, which can solve the problems of large solvent consumption, expensive equipment, and long time-consuming column chromatography for multiple separations, so as to reduce the amount of reagents, consume less, and increase the cost. The effect of large sample volume

Active Publication Date: 2018-07-06
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Among these three methods, multiple separations by column chromatography take a long time, high-speed countercurrent chromatography and preparative HPLC equipment are expensive, and solvent consumption is large

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Mix 18g of titanium dioxide, 450ml of toluene and 18g of amine stearate, stir and heat up to 90°C for 4 hours, and dry to obtain surface-modified TiO 2 ;

[0034] (2) Add 6g of sodium chloride, 2g of gelatin and 250ml of deionized water into a three-necked round-bottomed flask equipped with a thermometer, a stirrer, and a condensing reflux tube, heat up to 56°C, and stir for 2 hours to obtain a mixture containing sodium chloride and gelatin. The dispersed phase aqueous solution;

[0035] (3) 1g of surface-modified TiO 2 Mix with 100ml GMA, 12ml DVB, 0.5g BPO, 45ml toluene and 4.5ml n-heptane, stir until uniform to obtain a polymer phase solution;

[0036] (4) Mix the dispersed phase solution prepared in step 2 with the polymerized phase solution prepared in step 3 at a volume ratio of 2:1, stir and react at 55°C for 3h, then continue to stir and heat up to 80°C for 10h to solidify and wash , dried to get GMA / TiO 2 Copolymer microspheres, then the copolymer micro...

Embodiment 2

[0040] (1) Mix 16g of titanium dioxide, 400ml of toluene and 16g of amine stearate, stir and raise the temperature to 85°C for 5 hours, and dry to obtain surface-modified TiO 2 ;

[0041] (2) Add 8g of sodium chloride, 2g of gelatin, and 250ml of deionized water into a three-neck round-bottomed flask equipped with a thermometer, a stirrer, and a condensing reflux tube, heat up to 60°C, and stir for 2 hours to obtain a mixture containing sodium chloride and gelatin. The dispersed phase aqueous solution;

[0042] (3) 1g of surface-modified TiO 2 Mix with 100ml GMA, 10ml DVB, 0.3g BPO, 45ml toluene and 5ml n-heptane, stir until uniform to obtain a polymer phase solution;

[0043] (4) Mix the dispersed phase solution prepared in step 2 with the polymerized phase solution prepared in step 3 at a volume ratio of 3:1, stir and react at 55°C for 3h, then continue to stir and heat up to 85°C for 8h to solidify and wash , dried to get GMA / TiO 2 Copolymer microspheres, then the copol...

Embodiment 3

[0052] Weigh 30g of punicalagin with a purity of 45%, purify it with 600ml BUCT-1-1 filler, load the sample at a speed of 1.3 column volume / h, the loading concentration is 10mg / ml, the eluent is 5% ethanol, and use 2.6 column Volume / h flow rate elution, take the part of the 2-4th column volume of the eluate and spin dry to obtain punicalagin of 75%. Dry the obtained 75% punicalagin, take 4g of the mixed solution dissolved in 10ml scheme 1, the mixed solution of methanol, acetone and ethyl acetate (volume ratio is 20:55:22), and add the supernatant after centrifugation Chloroform, the volume percentage of chloroform in the mixed solution is 6%, and the supernatant after centrifugation is put into a refrigerator at 4° C. for two days. The precipitated punicalagin is centrifuged and dried to obtain the punicalagin product with a purity of 97%.

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Abstract

The invention relates to a method for preparing high-purity punicalagin crystal powder. The method disclosed by the invention comprises the steps: firstly, preparing TiO2 compound copolymer microspheres which have a function of separating a polar organic compound efficiently and effectively separating an organic compound with polyhydroxyl in a natural product; then initially purifying a punicalagin crude product with a mass fraction as 20 to 40% to 75 to 80% by utilizing the TiO2 compound copolymer microspheres as filler and utilizing an ordinary-pressure chromatography, wherein processing flux is large and consumed time is short; finally, utilizing the certain amount of methyl alcohol, acetone, diethyl ether and ethyl acetate mixed solution to dissolve a purified punicalagin sample, adding trichloromethane, centrifuging to take supernatant, putting in 4 DEG C environment and crystallizing to obtain punicalagin crystal with a purity as 97 to 98%. According to the method disclosed by the invention, the crystallizing method is utilized for the first time to obtain high-purity punicalagin crystal powder; the technology is simple, organic solvent consumption is small, sample processingflux is large, and consumed time is short; furthermore, required equipment cost is low, the problem of industrially preparing the high-purity punicalagin crystal is solved, and the method can be industrially popularized.

Description

technical field [0001] The invention relates to the preparation of high-purity punicalagin, in particular to the first use of physical methods to prepare high-purity punicalagin crystalline powder, which can meet the needs of industrial production. Background technique [0002] Punicalagin is a hydrolyzable tannin mainly found in pomegranate peel, with multiple phenolic hydroxyl groups in its structure, and its molecular formula is C 48 h 27 o 30 , molecular weight 1084.72. There is a pair of isomers of punicalagin, namely α-punicalagin and β-punicalagin, and the two can be converted into each other. The solid of punicalagin is green-yellow powder, easily soluble in water, soluble in methanol, ethanol, acetonitrile and other organic solvents. It will be degraded in case of acid, alkali and high temperature, and the degradation products include pomegranate, ellagic acid and so on. Picalagin is not easily synthesized and can only be extracted naturally at present. Picala...

Claims

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Application Information

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IPC IPC(8): C07H13/08C07H1/06C08F220/32C08F212/36C08J9/28B01J19/30
CPCB01J19/30C07H1/06C07H13/08C08F220/32C08F220/325C08J9/28C08J2333/14C08F212/36
Inventor 袁其朋徐巧莲李思彤
Owner BEIJING UNIV OF CHEM TECH
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