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Preparation method of crystallized apramycin sulfate

A technology of apramycin sulfate and apramycin, applied in the chemical field, can solve problems such as impurity of product components and impact on product quality, and achieve the effects of easy control, product quality assurance, and improved therapeutic effect

Active Publication Date: 2013-01-09
山东齐发药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The prior art prepares apramycin sulfate, except that a large amount of energy will be consumed in the production process, and because the spray drying method is adopted at last, all components in the solution all enter the final finished product, resulting in impure product components, which is harmful to the product. Quality affects

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1. Take 500ml of 380,000 U / ml apramycin concentrate, add 500ml of anhydrous salt water to dilute, add 1g of sodium bisulfite during the dilution process, adjust the pH to 5.7 with 10M sulfuric acid, and obtain 1025ml of salt solution, add activated carbon 10.25g (volume-to-mass ratio of salt-forming solution to activated carbon: 1%, g / ml), fully stirred for 60 minutes, and filtered to obtain the filtrate.

[0026] 2. Take 4100ml of ethanol with a volume percentage concentration of 95%, and under the crystallization temperature of 18-20°C, slowly and uniformly add the filtrate obtained in step 1, and stir fully during the process. After the addition, stir for 30 minutes, there is Apramycin sulfate Suction crystals were precipitated, filtered to obtain a wet product, rinsed with 50ml of ethanol, and suction filtered under reduced pressure.

[0027] 3. Dry for 3 hours under the conditions of vacuum degree 0.06MPa and temperature 60-65°C to obtain 310g of crystals with a me...

Embodiment 2

[0029] Take 500ml of 420,000 U / ml apramycin concentrate, add 600ml of anhydrous salt water to dilute, add 1.1g of sodium bisulfite during the dilution process, adjust the pH to 5.7 with 10M sulfuric acid, and obtain 1140ml of salt-forming solution, add 11.40g activated carbon, fully stirred for 60 minutes, and filtered to obtain the filtrate. Take 4560ml of 95% ethanol, under the condition of crystallization temperature of 15-18°C, slowly add the filtrate obtained in the previous step at a uniform speed, fully stir during the process, after the addition, stir for 30 minutes, filter, and obtain the wet product of crystallization, use 50ml of ethanol Rinse and filter under reduced pressure. Dry for 3 hours under the conditions of vacuum degree 0.08MPa and temperature 60-65°C to obtain 335g of finished product with a content of 625U / mg.

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Abstract

The invention relates to a preparation method of crystallized apramycin sulfate, which comprises the steps of: with an apramycin concentrated solution as a raw material, blending a feed solution, salifying and crystallizing, drying and the like. The concentration of the feed solution is regulated to a certain range, filtrate is added in alcohol quantitatively under the stirring, the crystallizingtemperature is controlled, therefore, most of impurities in the feed solution are removed, and the crystallized apramycin sulfate with good graininess and purer component is obtained.

Description

technical field [0001] The invention relates to a preparation method of crystalline apramycin sulfate, which belongs to the technical field of chemistry. Background technique [0002] Apramycin sulfate is a kind of antibiotic raw material drug. At present, the preparation of pure apramycin sulfate generally adopts the spray drying method. Adsorbed from the medium, and then desorbed to obtain apramycin solution. The solution is concentrated, added sulfuric acid to form a salt, and adsorbed by activated carbon. It is atomized by a high-speed feed pump and heated by high-temperature air to remove moisture to obtain a product. The finished product is yellow Brown homogeneous powder. The final step of preparing pure apramycin sulfate generally adopts the spray drying method. The prior art prepares apramycin sulfate, except that a large amount of energy will be consumed in the production process, and because the spray drying method is adopted at last, all components in the solut...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H15/224C07H1/00
Inventor 丁新仁程宏张效军
Owner 山东齐发药业有限公司
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