Astaxanthin methoxy polyethylene glycol acetate and preparation method thereof
A technology of methoxy polyethylene glycol and astaxanthin acetate, applied in the field of methoxy polyethylene glycol astaxanthin acetate and preparation thereof, can solve the problem of poor water dispersibility, inability to fully play a role, and astaxanthin It is easy to aggregate and other problems, and achieves the effects of mild reaction conditions, good water solubility and simple process.
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Embodiment 1
[0034] Synthesis: 40mg of free astaxanthin, 1 times the molar amount of methoxypolyethylene glycol acetic acid (mPEG-CM, molecular weight about 2000), 200mg of DMAP, put into a 100ml serum bottle, add 30ml of dichloromethane and stir to dissolve; nitrogen, protected from light, and shaken for 12 hours in a constant temperature incubator (100 rpm / min) at 37°C. The synthesis rate of mPEG-CM@AST can reach 90.62%.
[0035]Purification: remove the organic solvent by rotary evaporation under reduced pressure, redissolve with 80ml of dichloromethane, wash with 200ml of hydrochloric acid solution (1mol / l), 200ml of saturated sodium bicarbonate solution, and 200ml of saturated sodium chloride solution for 3 times in sequence; anhydrous sulfuric acid Sodium in addition to water. The organic phase was recovered and rotary evaporated to dryness to obtain a crude product. A small amount of the crude product was removed and redissolved in chromatographically pure dichloromethane for TLC an...
Embodiment 2
[0037] Synthesis: 80mg of free astaxanthin, 1 times the molar amount of methoxypolyethylene glycol acetic acid (mPEG-CM, molecular weight about 2000), 150mg of EDCI, put into a 100ml serum bottle, add 25ml of acetone, fill with nitrogen, and avoid light , shaking in a constant temperature incubator (100rpm / min) at 30°C for 6h.
[0038] Purification: remove the organic solvent by rotary evaporation under reduced pressure, redissolve with 120ml of dichloromethane, wash with 350ml of hydrochloric acid solution (1mol / l), 350ml of saturated sodium bicarbonate solution, and 350ml of saturated sodium chloride solution for 3 times in sequence; anhydrous sulfuric acid Sodium in addition to water. The organic phase was recovered and rotary evaporated to dryness to obtain a crude product. A small amount of the crude product was removed and redissolved in chromatographically pure dichloromethane for TLC and HPLC detection.
Embodiment 3
[0040] Synthesis: 40mg of free astaxanthin, 4 times the molar amount of methoxypolyethylene glycol acetic acid (mPEG-CM, molecular weight about 5000), 250mg of triethylamine, put into a 100ml serum bottle, add 35ml of ethyl acetate, fill nitrogen, protected from light, and shaken for 18 hours in a constant temperature incubator (100 rpm / min) at 25°C.
[0041] Purification: Remove the organic solvent by rotary evaporation under reduced pressure, then redissolve with 200ml of dichloromethane, wash with 450ml of hydrochloric acid solution (1mol / l), 450ml of saturated sodium bicarbonate solution, and 450ml of saturated sodium chloride solution for 3 times in sequence; anhydrous sulfuric acid Sodium in addition to water. The organic phase was recovered and rotary evaporated to dryness to obtain a crude product. A small amount of the crude product was removed and redissolved in chromatographically pure dichloromethane for TLC and HPLC detection.
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