A method for preparing punicalagin crystalline powder

A technology of punicalagin and crystalline powder, which is applied in the field of preparation of high-purity punicalagin, and can solve problems such as expensive equipment, large solvent consumption, and long time-consuming column chromatography for multiple separations.

Active Publication Date: 2020-10-27
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 raise the temperature to 90℃ to react for 4h, 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, agitator, and condenser reflux tube, heat to 56°C, stir for 2h, and obtain sodium chloride and gelatin The dispersed phase aqueous solution;

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

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

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 to react for 5h, 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-necked round bottom flask equipped with a thermometer, agitator, and reflux tube, heat to 60°C, stir for 2h, and obtain sodium chloride and gelatin. The dispersed phase aqueous solution;

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

[0043] (4) Mix the dispersed phase solution prepared in step 2 with the polymer phase solution prepared in step 3 in a volume ratio of 3:1, stir and react at 55°C for 3 hours, and then continue to stir and warm up to 85°C for 8 hours to solidify and wash , Dry to get GMA / TiO 2 Copolymer microspheres, then add the copolymer microspheres to dry N,N-dimethylfo...

Embodiment 3

[0052] Weigh 30g of punicalagin with a purity of 45%, purify it with 600ml BUCT-1-1 packing, load the sample at a speed of 1.3 column volume / h, and load the sample at a concentration of 10mg / ml. The eluent is 5% ethanol. Volume / h flow rate elution, take the 2-4 column volume part of the eluate and spin dry to obtain 75% punicalagin. Dry the obtained 75% punica granatum, take 4g dissolved in 10ml of the mixed solution in Scheme 1, a mixed solution of methanol, acetone and ethyl acetate (volume ratio 20:55:22), add the supernatant after centrifugation Trichloromethane, the volume percentage of chloroform in the mixed solution is 6%, and the supernatant is placed in a refrigerator at 4°C for two days after centrifugation. Centrifugal drying the precipitated punicalagin can obtain a 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 physical method to prepare high-purity punicalagin crystalline powder, which can meet the requirements of industrial production. Background technique [0002] Punicalagin is a hydrolyzable tannin mainly found in pomegranate peel. Its structure contains multiple phenolic hydroxyl groups. Its molecular formula is C 48 H 27 O 30 , The molecular weight is 1084.72. There are a pair of isomers of punica granatum, namely α-puunicalarin and β-puunicalarin, and the two can be converted to each other. The solid of punicalagin is a green-yellow powder, easily soluble in water, soluble in various organic solvents such as methanol, ethanol and acetonitrile. It is degraded when exposed to acid, alkali and high temperature, and the degradation products include Anguolin and ellagic acid. Punicaridin is not easy to be synthesized and can only be extracted naturally. Punicarin ...

Claims

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Application Information

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