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A kind of acidic cationic resin purification prepares the method for amikacin sulfate

A technology of amikacin sulfate and acid cation, applied in the field of medicine, can solve the problems of difficult recovery, high odor of ammonia water, small adsorption capacity, etc., and achieve the effect of ensuring the effect of separation and purification

Active Publication Date: 2022-03-22
山东安信制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses ammonia water as the eluent, which has the disadvantages of small adsorption capacity, strong ammonia smell, and difficult recovery, which increases the cost of waste water, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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PUM

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Abstract

The invention discloses a method for purifying and preparing amikacin sulfate by acidic cationic resin. In the present invention, the feed liquid containing amikacin is placed on a weakly acidic cationic resin column, and then a 5%-10% ammonium sulfate solution is used for gradient release. is eluted out, then obtains amikacin sulfate feed solution, and finally elutes the impurities with strong binding force, and the obtained amikacin sulfate feed liquid is concentrated and directly added with methanol to crystallize to obtain amikacin sulfate, the mother liquor Continue to add methanol to separate out ammonium sulfate, which can be recycled. Using ammonium sulfate solution as the release agent, the collected amikacin feed solution is the amikacin sulfate solution, and there is no need to add sulfuric acid to form a salt. The method is simple and environmentally friendly.

Description

technical field [0001] The invention relates to a method for purifying and preparing amikacin sulfate by acidic cationic resin, which belongs to the technical field of medicine. Background technique [0002] Amikacin is a semi-synthetic aminoglycoside antibiotic with a broad antibacterial spectrum and strong antibacterial ability against a variety of bacteria. Since its launch in the 1970s, amikacin has been widely used due to its definite curative effect and has become a commonly used first-line anti-infective drug in the world. [0003] The synthesis method of amikacin commonly used at present: (1) kanamycin A and hexamethyldisilazane take place silylation reaction, the hydrogen atom on the amino group and the hydroxyl group of kanamycin A is replaced by trimethylsilyl Substitution generates kanamycin A silylate; (2) PHBA and NOP undergo an esterification reaction under the action of DCC dehydrating agent to generate active ester; (3) active ester and silylate undergo acy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H1/06C07H15/234
CPCC07H1/06C07H15/234
Inventor 翟长均蔡成伟孟令华李东建王晓然张丽
Owner 山东安信制药有限公司
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