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A kind of preparation method of dihydrostreptomycin sulfate

A technology of dihydrostreptomycin sulfate and streptomycin sulfate, which is applied in the preparation of sugar derivatives, chemical instruments and methods, organic chemistry, etc., and can solve the problems of low utilization rate of reducing agent, high consumption of oxalic acid, large power consumption, etc. problem, to achieve the effect of increasing the amount of decolorizing agent, high purity and improving utilization rate

Active Publication Date: 2019-06-28
华北制药华胜有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The electrolytic reduction method is to place streptomycin in the cathode tank, and reduce it by applying an appropriate current, but this method consumes a large amount of electric energy, and the reaction efficiency is low
[0004] The production of dihydrostreptomycin by reduced hydrogen reduction method can be carried out under normal temperature and pressure, but the existing preparation process generally has high consumption of oxalic acid, low utilization rate of reducing agent, poor product purity, low pass rate and unstable quality, etc. question

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  • A kind of preparation method of dihydrostreptomycin sulfate

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preparation example Construction

[0041] A kind of preparation method of dihydrostreptomycin sulfate of the present invention, its specific implementation steps are as follows:

[0042] a. According to 6 ~ 16kg / m 3 Add oxalic acid to the streptomycin fermentation broth, then adjust the pH to 2.5-3.5 with sulfuric acid, heat to 60-85°C, remove insoluble matter by centrifugation or filtration, and then adjust the pH to 7.0-8.5 with sodium hydroxide, Prepare streptomycin stock solution;

[0043] b. Adsorb and saturate the streptomycin stock solution with sodium type 110 resin, D152 resin or D150 resin, wash with soft water, anhydrous salt water or purified water, and then elute with 5.0-6.5% dilute sulfuric acid to obtain streptomycin sulfate eluent;

[0044] c. Adsorb and saturate the streptomycin eluate with macroporous primary amine-based resin D303, wash with anhydrous brine or purified water and press dry, and then use 7.0-9.0% dilute sulfuric acid to circulate and analyze to obtain streptomycin sulfate a...

Embodiment 1

[0054] A kind of preparation method of dihydrostreptomycin sulfate of the present embodiment, its specific implementation steps are as follows:

[0055] a. According to 6kg / m 3 Add oxalic acid to streptomycin fermentation broth, then adjust pH to 2.5 with sulfuric acid, heat to 60°C, remove insoluble matter by centrifugation or filtration, and then adjust pH to 7.0 with sodium hydroxide to obtain streptomycin stock solution ;

[0056] b. After the streptomycin stock solution is adsorbed and saturated with sodium type 110 resin, it is washed with soft water and pressed dry, and then eluted with 5.0% dilute sulfuric acid to obtain a streptomycin sulfate eluent;

[0057] c. Absorb and saturate the streptomycin eluate with macroporous primary amine-based resin D303 or D318, wash with purified water, and then analyze with 8.0% dilute sulfuric acid to obtain a streptomycin sulfate analysis solution;

[0058] d. After adjusting the pH of the streptomycin sulfate analysis solution t...

Embodiment 2

[0067] A kind of preparation method of dihydrostreptomycin sulfate of the present embodiment, its specific implementation steps are as follows:

[0068] a. According to 16kg / m 3 Add oxalic acid to streptomycin fermentation broth, then adjust pH to 3.5 with sulfuric acid, heat to 85°C, remove insoluble matter by centrifugation or filtration, and then adjust pH to 8.5 with sodium hydroxide to obtain streptomycin stock solution ;

[0069] b. After the streptomycin stock solution is adsorbed and saturated with sodium D152 resin, it is washed with anhydrous brine and eluted with 5.0% dilute sulfuric acid to obtain a streptomycin sulfate eluent;

[0070] c. The streptomycin eluate was absorbed and saturated with macroporous primary amine-based resin D318 resin, washed with anhydrous brine and pressed dry, and then analyzed with 6.0% dilute sulfuric acid to obtain a streptomycin sulfate analysis solution;

[0071]d. After adjusting the pH of the streptomycin sulfate analysis soluti...

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Abstract

The invention discloses a preparation method for dihydrostreptomycin sulphate and belongs to the production preparation technology of semi-synthesis antibiotics. The method comprises the following steps: treating with acid; performing ion exchange; adsorbing with large-pore amino resin; hydrogenating; performing secondary ion exchange; purifying by a mixed bed; treating with activated carbon; concentrating through a nanofiltration membrane; decolorizing by activated carbon; and treating with an ultrafiltration membrane and performing spray drying. According to the invention, the dosage of oxalic acid in a preparation process is reduced, the use ratio of the reducing agent is increased, the production cost is lowered, the production efficiency is increased, the method can meet the industrial production requirement and the product purity, quality yield and total recovery of the dihydrostreptomycin sulphate are increased.

Description

technical field [0001] The invention relates to a preparation method of a compound, in particular to a preparation method of dihydrostreptomycin sulfate, which belongs to the production and preparation process of semi-synthetic antibiotics. Background technique [0002] Streptomycin is an alkaline antibiotic isolated from the culture solution of Streptomyces griseus by Selman Waxman in 1944. It has anti-conjugated bacillus properties and can also be used as a bactericidal agent in veterinary drugs and pesticides agent. Its molecular structure is composed of three parts of streptavidin, streptomycin and N-methyl-L-glucosamine connected by glycoside bonds, and the molecular formula is C 21 h 39 N 7 o 12 . Dihydrostreptomycin sulfate is to hydrogenate the aldehyde group of streptomycin and reduce it to alcoholic hydroxyl group, and convert it into sulfate form, which can well overcome the problem of poor stability of streptomycin, and its antibacterial spectrum is similar ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H15/238C07H1/06
CPCC07H1/06C07H15/238
Inventor 武仲涛郝宝员任刚孙丙林张伟贾啸静程曜峰张志江张天兵彭敬梅
Owner 华北制药华胜有限公司
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