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Preparation method of acetylisovaleryltylosin tartrate

A technology for acetylisovaleryl tylosin tartrate and acetylisovaleryl tylosin is applied in the field of preparation of acetylisovaleryl tylosin tartrate, and can solve the problems of high operation toxicity, difficulty in filtration, environmental pollution and the like , to avoid environmental pollution problems, reduce the introduction of impurities, and improve the extraction yield.

Active Publication Date: 2014-07-16
宁夏泰瑞制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 1) Extraction method: the extraction method uses organic solvent as the extraction agent for extraction. This process ① is prone to emulsification during the production process; ② the operation is highly toxic and easy to pollute the environment; ③ the production cost is high, which is not conducive to large-scale Production; ④ low yield, generally only about 80%
[0005] 2) Secondary crystallization method and salting-out method: At present, domestic super tylosin manufacturers generally use secondary crystallization method or salting-out method to extract super tylosin. ② the crystallization effect is poor, the crystals are finely broken, and it is difficult to filter; ③ the production cost is high, which is not conducive to large-scale production; ④ the yield is low, generally only 85-90 %

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The titer of the acetylisovaleryl tylosin fermentation broth is 16479μ / ml, and the volume of the fermentation broth is 5m 3 .

[0036] Acidify the acetylisovaleryl tylosin fermentation broth, adjust the pH to 1.1 with oxalic acid and let it stand for 20 minutes, then continue to adjust the pH to 4.5 with 10% liquid alkali and let it stand for 20 minutes.

[0037] The acetylisovaleryl tylosin fermentation broth was heated up to 40°C, and plate and frame filtration was performed, and the material of the filter cloth was polyester. Filtration ends, obtain filtrate 4.6m 3 , the titer was 17249μ / ml, and the yield of pretreatment was 96.3%.

[0038] Dilute acetylisovaleryl tylosin fermentation broth to 14m with drinking water 3 .

[0039] At 40°C, a mixture of 14kg of activated carbon and 280kg of potassium chloride was added, and the stirring and standing time were controlled at 20min, respectively. Carry out solid-liquid separation after decolorization, obtain filtrate...

Embodiment 2

[0047] The titer of the acetylisovaleryl tylosin fermentation broth is 15637μ / ml, and the volume of the fermentation broth is 5m 3 .

[0048] Acidify the acetylisovaleryl tylosin fermentation broth, adjust the pH to 1.2 with oxalic acid and let it stand for 23 minutes, then continue to adjust the pH to 4.7 with 12% liquid alkali and let it stand for 23 minutes.

[0049] The acetylisovaleryl tylosin filtrate was warmed up to 42°C, and subjected to plate and frame filtration, and the material of the filter cloth was polypropylene fiber. Filtration ends, obtain filtrate 4.6m 3 , the titer was 16385μ / ml, and the yield of pretreatment was 96.4%.

[0050]Dilute acetylisovaleryl tylosin filtrate to 16.1m with drinking water 3 .

[0051] At 42°C, a mixture of 24kg of diatomaceous earth and 400kg of sodium chloride was added, and the stirring and standing time were respectively controlled at 22min. Carry out solid-liquid separation after decolorization, obtain filtrate 16m 3 , th...

Embodiment 3

[0059] The titer of the acetylisovaleryl tylosin fermentation broth is 15862μ / ml, and the volume of the fermentation broth is 5m 3 .

[0060] Acidify the acetylisovaleryl tylosin fermentation broth, adjust the pH to 1.3 with oxalic acid and let it stand for 25 minutes, then continue to adjust the pH to 5 with 13% liquid alkali and let it stand for 25 minutes.

[0061] The acetylisovaleryl tylosin fermentation broth was heated up to 45°C, and plate-and-frame filtration was performed, and the material of the filter cloth was polyester. Filtration ends, obtain filtrate 4.6m 3 , the titer was 16707μ / ml, and the yield of pretreatment was 96.9%.

[0062] Dilute acetylisovaleryl tylosin filtrate to 18.4m with drinking water 3 .

[0063] At 45°C, a mixture of 31.6kg of activated carbon and 552kg of potassium chloride was added, and the stirring and standing time were respectively controlled at 25min. After decolorization, solid-liquid separation was carried out to obtain a filtra...

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Abstract

The invention relates to a preparation method of acetylisovaleryltylosin tartrate. The method comprises the following steps: adjusting the pH of acetylisovaleryltylosin fermentation liquor to 1-1.5 by using oxalic acid, and standing for 20-30 minutes; adjusting the pH of acetylisovaleryltylosin back to 4.5-5.5 by using 10-15 percent liquid alkali; standing for 20-30 minutes once again; performing plate frame filtering, diluting, decolorizing, nano-filtering, crystalizing, water washing, salifying and spray drying on the fermentation liquor to obtain the acetylisovaleryltylosin tartrate. By adopting the preparation method, the conventional crystallizing process is eliminated, the yield of acetylisovaleryltylosin tartrate is increased by virtue of extracting, crystallizing and synthesizing processes, the cost is lowered, and the product quality is improved. The method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of antibiotic extraction and synthesis, and in particular relates to a preparation method of acetylisovaleryl tylosin tartrate. Background technique [0002] Tylosin acetylisovaleryl tartrate, also known as super tylosin, is a kind of macrolide antibiotics specially used for livestock and poultry which is semi-synthesized on the basis of tylosin through biological fermentation. As a new type of macrolide antibiotics, it overcomes the shortcomings of many macrolides, and has the characteristics of high efficiency, broad spectrum, less resistance, and less toxic side effects. It is a good antibiotic for digestive system diseases and has broad application prospects. [0003] Tylos acetylisovaleryl is a weak base and can form salts with tartaric acid, etc. Utilizing its physical and chemical properties, its extraction process has been reported in China. The main methods include organic solvent extraction, seco...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08C07H1/06
Inventor 任勇
Owner 宁夏泰瑞制药股份有限公司
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