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Preparation method of tylosin

A technology of tylosin and tylosin tartrate, which is applied to the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of unusable, ineffective removal of impurities, and low content of tylosin A and other issues to achieve the effect of improving product purity

Inactive Publication Date: 2019-03-29
NINGXIA TAIYICIN BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the process is simple to operate and the production cycle is short, it cannot effectively remove impurities, resulting in too low content of tylosin A and cannot be used

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Take 5m of the refined solution of tylosin tartrate 3 , the titer is 193788U / ml. Use 30% NaOH solution to adjust the pH to 9.3. After a large amount of crystallization, grow crystals for 1.5 hours until tylosin is fully separated, and obtain a filter cake by solid-liquid separation. After the filter cake is washed with purified water, it is properly dried to obtain crude tylosin. .

[0017] Add dichloromethane 2.9m to the above-mentioned tylosin crude product 3 , heated to 35°C to dissolve and make a nearly saturated solution, and filtered while hot to remove insoluble impurities to obtain a filtrate.

[0018] Cool the above filtrate to 11°C, stir and keep it warm for 2 hours, centrifuge to remove the supernatant, and dry the crystals to obtain tylosin. The yield was 98.9%, and the content of component A was 97.7%.

Embodiment 2

[0020] Take 5m of the refined solution of tylosin tartrate 3 , the titer is 250291U / ml. Use 30% NaOH solution to adjust the pH to 10.7, grow a large amount of crystals, grow crystals for 2 hours until tylosin is fully separated, and obtain a filter cake by solid-liquid separation. After the filter cake is washed with purified water, it is properly dried to obtain crude tylosin.

[0021] Add 5.0 m of dichloromethane to the crude product of tylosin 3 , heated to 40°C to dissolve and make a nearly saturated solution, and filter while hot to remove insoluble impurities to the filtrate.

[0022] Cool the above filtrate to 10°C, stir and keep it warm for 2.5 hours, centrifuge to remove the supernatant, and dry the crystals to obtain tylosin. The yield was 98.6%, and the content of component A was 98.1%.

Embodiment 3

[0024] Take 5m of the refined solution of tylosin tartrate 3 , the titer is 297873U / ml. Use 30% NaOH solution to adjust the pH to 11.0. After a large amount of crystallization, grow crystals for 3 hours until tylosin is fully separated, and obtain a filter cake by solid-liquid separation. After the filter cake is washed with purified water, it is properly dried to obtain crude tylosin.

[0025] Add dichloromethane 6.7m to the above-mentioned tylosin crude product 3 , heated to 38 ° C to dissolve and make a nearly saturated solution, and filter while hot to remove insoluble impurities to the filtrate.

[0026] Cool the above filtrate to 12°C, stir and keep it warm for 3 hours, centrifuge to remove the supernatant, and dry the crystals to obtain tylosin. The yield was 99.0%, and the content of component A was 98.3%.

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PUM

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Abstract

The invention relates to a preparation method of tylosin. The process comprises the following steps: adjusting a tylosin tartrate refined liquid to be alkaline, carrying out solid-liquid separation astylosin is fully separated out, washing obtained filter cakes with purified water, and performing drying to obtain a tylosin crude product; and dissolving the crude tylosin product with dichloromethane with heating to obtain a nearly-saturated solution, filtering the solution when the solution is hot to remove insoluble impurities, and subjecting the filtrate to cooling, crystallization and separation. Compared with the prior art, the method has increased steps, but can effectively remove impurities in the product, and improve the purity of the product and the content of tylosin A in the product. Experiments prove that the content of the component A in the tylosin product is up to 97.0% or above, and the yield is up to 96.0% or above.

Description

technical field [0001] The invention belongs to the technical field of antibiotic refining, and in particular relates to a preparation method of tylosin. Background technique [0002] Tylosin is a macrolide antibiotic obtained by fermenting and extracting actinomycetes Streptomyces freundii. It is mainly used as an animal-specific antibiotic and is the world-recognized first-choice drug for the treatment and prevention of mycoplasma infection in livestock and poultry. Tylosin is a mixture of four components A, B, C, and D, among which: A component is Tylosin (Tylosin), B component is decarbosugar Tylosin (Desmycosin) , C group is Macrosin (Macrosin), D group is Relomycin (Relomycin) and the structural analogue Laktin. Among the above four components, other groups except D component Relomycin All components have antibacterial activity in the test tube, and the component of tylosin A has been confirmed to have higher activity in vivo. Therefore, the content of tylosin A is us...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08C07H1/00C07H1/06
CPCC07H1/00C07H1/06C07H17/08
Inventor 梁丽娟
Owner NINGXIA TAIYICIN BIOTECH CO LTD