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.
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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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