Method for preparing amikacin sulfate by purifying acidic cationic resin
A technology of amikacin sulfate and acidic cations, which is applied in the field of medicine, can solve the problems of difficult recovery, strong ammonia odor, and small adsorption capacity, and achieve the effect of ensuring the effect of separation and purification
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Embodiment 1
[0026] Take 518ml of the amikacin solution to be purified, with an optical rotation of 11°, put it on a 4L CD180 resin column, wash it with 4L of water after adsorption, and elute with a gradient of 5%-10% ammonium sulfate solution, and use 5%, 7%, and 9% sulfuric acid in sequence Ammonium solution elution, the elution speed is 30ml / min, 5% ammonium sulfate releases the components before amikacin, 7% ammonium sulfate solution amikacin sulfate feed liquid, 9% ammonium sulfate solution elutes Impurities remain in the column, washed with water until the concentration of ammonium sulfate solution is <5%.
[0027] Concentrate the amikacin sulfate feed solution until the optical rotation is 70 °, add 0.5 times the volume of methanol to the amikacin sulfate feed solution obtained above, stir and crystallize for 2 hours, filter with suction, wash with 30%-40% methanol, and dry Dry to obtain 20.0 g of amikacin sulfate, the liquid phase purity is 99.8%, and the single impurity is <0.1%....
Embodiment 2
[0029] Take 518ml of amikacin solution to be purified, with an optical rotation of 11°, put it on a 4L CD180 resin column, wash it with 4L of water after adsorption, and elute with a gradient of 5%-10% ammonium sulfate solution, and use 6%, 8%, and 10% sulfuric acid in sequence Ammonium solution elution, the elution rate is 30ml / min, 6% ammonium sulfate releases the components before amikacin, 8% ammonium sulfate solution amikacin sulfate feed liquid, 10% ammonium sulfate solution elutes Impurities remain in the column, washed with water until the concentration of ammonium sulfate solution is <5%.
[0030] Concentrate the amikacin sulfate feed solution until the optical rotation is 80 °, add 0.5 times the volume of methanol to the amikacin sulfate feed solution obtained above, stir and crystallize for 2 hours, filter with suction, wash with 30%-40% methanol, and dry 19.8 g of amikacin sulfate was obtained by drying, the liquid phase purity was 99.9%, and individual impurities ...
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