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Preparation method of crystalline particles of acetyl isovaleryl tylosin salt

A technology of acetylisovaleryl tylosin and crystalline granules, which is applied in the field of preparation of acetylisovaleryl tylosin salt crystalline granules, can solve the problems of affecting normal use, small powder specific gravity, slow dissolution, etc., to reduce pollution, Not easy to agglomerate, fast dissolution effect

Active Publication Date: 2013-09-04
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

The powder produces a lot of dust during the packaging process, causing certain harm to the operator's body and causing certain pollution to the environment; use acetylisovaleryl tylosin salt powder to add to feed or drinking water for animals, and the specific gravity of the powder is small , floating on the water, dissolving slowly, affecting normal use
Some companies sell acetylisovaleryl tylosin salt as premixes or granules, but the content will be reduced during the preparation process, which will affect the efficacy of the medicine

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh 10 kg of acetylisovaleryl tylosin tartrate powder, and measure 30 L of ethyl acetate. Start the stirring system, add acetylisovaleryl tylosin tartrate into ethyl acetate, and then lower the temperature to 2°C. The speed is controlled at 20r / min. Slowly add isobutanol while stirring, the amount of isobutanol added is 30L, the rate of addition is controlled at 10% / min of the total amount, and the temperature is always controlled at 0-2°C throughout the mixing process. After mixing, let stand for 30 minutes for solid-liquid separation. The solid obtained after centrifugation was rinsed twice with isobutanol at 2° C., the amount used for the first rinse was 15 L, and the amount used for the second rinse was 15 L. Start the double-cone rotary vacuum dryer to dry, the drying temperature is controlled at 50°C, the vacuum degree is controlled at -0.02MPa, until the weight loss on drying is less than 1%, 9.82kg of acetylisovaleryl tartrate crystalline particles of tylosi...

Embodiment 2

[0026] Weigh 10 kg of acetylisovaleryl tylosin tartrate powder, and measure 40 L of ethyl acetate. Start the stirring system, add acetylisovaleryl tylosin tartrate into ethyl acetate, and then lower the temperature to 1°C. The speed is controlled at 25r / min. Slowly add isobutanol while stirring, the amount of isobutanol added is 60L, the dropping rate is controlled at 10% / min of the total amount, and the temperature is always controlled at 0-2°C during the whole mixing process. After mixing, let stand for 30 minutes for solid-liquid separation. The solid obtained after centrifugation was rinsed twice with isobutanol at 1° C., the amount used for the first rinse was 30 L, and the amount used for the second rinse was 30 L. Start the double-cone rotary vacuum dryer to dry, the drying temperature is controlled at 55°C, the vacuum degree is controlled at -0.02MPa, until the weight loss on drying is less than 1%, 9.84kg of tartrate acetylisovaleryl tylosin crystalline particles ar...

Embodiment 3

[0028] Weigh 10 kg of acetylisovaleryl tylosin tartrate powder, and measure 50 L of ethyl acetate. Start the stirring system, add acetylisovaleryl tylosin tartrate into ethyl acetate, and then cool down to 0°C. The speed is controlled at 30r / min. Slowly add isobutanol while stirring, the amount of isobutanol added is 100L, the rate of addition is controlled at 10% / min of the total amount, and the temperature is always controlled at 0-2°C throughout the mixing process. After mixing, let stand for 30 minutes for solid-liquid separation. The solid obtained after centrifugation was rinsed twice with isobutanol at 0° C., the amount used for the first rinse was 50 L, and the amount used for the second rinse was 50 L. Start the double-cone rotary vacuum dryer to dry, the drying temperature is controlled at 60°C, the vacuum degree is controlled at -0.02MPa, until the weight loss on drying is less than 1%, 9.87kg of tartrate acetylisovaleryl tylosin crystalline particles are obtained...

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Abstract

The invention relates to a preparation method of crystalline particles of acetyl isovaleryl tylosin salt. The method comprises the steps of sufficiently dissolving powder of the acetyl isovaleryl tylosin salt in ethyl acetate, slowly and dropwise adding isobutanol for mixing in a stirring state and at 0-2 DEG C, standing after the mixing, conducting solid-liquid separation, eluting, and conducting vacuum drying. According to the preparation method, the acetyl isovaleryl tylosin salt is prepared into the crystalline particles to replace powder; the specific gravity of the crystalline particles is greater, so that dust pollution is avoided in packaging and using processes; the crystalline particles are added to animal drinking water to sink into the water bottom, are better in dispersity, higher in dissolving speed and higher in content, and can be directly added to animal feed or the animal drinking water; a used organic solvent can be recovered and recycled; and the preparation method has a certain application prospect.

Description

technical field [0001] The invention belongs to the technical field of antibiotic product preparation, in particular to a method for preparing acetylisovaleryl tylosin salt crystal particles. Background technique [0002] Acetylisovaleryl tylosin, also known as tylosin, is a macrolide-type poultry-specific antibiotic obtained by semi-synthesizing on the basis of tylosin through biological fermentation. The production strain is heat-resistant chain A mutant strain of mold, belonging to a type of actinomycetes. 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. The salts of acetylisovaleryl tylosin are common in the market. [0003] At present, domestic manufacturers prepare acetylisovaleryl tylosin salt by spray drying to obtain solid po...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08C07H1/06A61K9/14A61P31/04
Inventor 任勇周丽娜
Owner 宁夏泰瑞制药股份有限公司
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