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Preparation method of tilmicosin phosphate crystal

A technology of tilmicosin phosphate and crystals, which is applied in the preparation of sugar derivatives, chemical instruments and methods, organic chemistry, etc., can solve the problems of reducing the content of tilmicosin phosphate, physical injury of operators, and affecting normal use, etc. Achieve the effects of reducing physical hazards, reducing pollution, and fast dissolution

Active Publication Date: 2013-09-11
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

During the production and packaging process, a large amount of dust pollution is likely to be generated, causing certain injuries to the operator; during use, tilmicosin phosphate is added to feed or drinking water for animals, and due to the small specific gravity of the powder, it floats on the water surface , dissolves slowly, affecting normal use
Some companies sell tilmicosin phosphate as premix or granules, but the content of tilmicosin phosphate will be reduced during the preparation process, resulting in reduced efficacy

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Weigh 10 kg of Tilmicosin phosphate powder, and weigh 30 L of ethyl acetate. Tilmicosin phosphate was added to ethyl acetate, stirring was started for dissolution, and the rotation speed was controlled at 20r / min. Then the temperature was lowered to 5°C, and isopropyl ether was slowly added under stirring. The amount of isopropyl ether added was 30L. When adding dropwise, the amount added per minute is controlled to be 1 / 10 of the total amount, the speed is controlled at 15r / min, and the temperature is always controlled at 0~5℃ during the whole process. At the end of the dropping, the stirring speed is controlled at 10r / min, and the stirring is continued for 1 hour. Use a centrifuge for solid-liquid separation. The solid obtained after centrifugation was washed twice with isopropyl ether at 5°C, the first rinse was 15L, and the second rinse was 15L. At a temperature of 50℃, using a double-cone rotary vacuum dryer, the vacuum degree is controlled at -0.02MPa, and the d...

Embodiment 2

[0023] Weigh 10 kg of Tilmicosin phosphate powder, and measure 40L of ethyl acetate. Tilmicosin phosphate was added to ethyl acetate, stirring was started to dissolve, and the rotation speed was controlled at 25r / min. Then lower the temperature to 3°C, slowly add isopropyl ether while stirring, the amount of isopropyl ether added is 60L, and the amount added per minute is controlled to be 1 / 10 of the total amount during dripping, and the speed is controlled at 25r / min. During the whole process The temperature is always controlled at 0~5℃. At the end of the dripping, the stirring speed is controlled at 10r / min, and the stirring is continued for 1h. Use centrifugal equipment for solid-liquid separation. The solid obtained after centrifugation was rinsed twice with isopropyl ether at 3°C, the first dose was 29L, and the second dose was 30L. At a temperature of 55°C, a double-cone rotary vacuum dryer was used, and the vacuum degree was controlled at -0.05MPa, until the drying we...

Embodiment 3

[0025] Weigh 10 kg of Tilmicosin phosphate powder, and weigh 50L of ethyl acetate. Tilmicosin phosphate was added to ethyl acetate, stirring was started to dissolve, and the rotation speed was controlled at 30r / min. Then lower the temperature to 0°C, slowly add isopropyl ether under stirring, the amount of isopropyl ether added is 100L, and the amount added per minute is controlled to be 1 / 10 of the total during the dripping, and the speed is controlled at 30r / min. During the whole process The temperature is always controlled at 0~5℃. At the end of the dropping, the stirring speed is controlled at 10r / min, and the stirring is continued for 1 hour. Use centrifugal equipment for solid-liquid separation. The solid obtained after centrifugation was washed twice with isopropyl ether at 0° C. The amount of isopropyl ether used for the first time was 48 L, and the amount of isopropyl ether used for the second time was 49 L. At a temperature of 60°C, a double-cone rotary vacuum drye...

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Abstract

The invention relates to a preparation method of a tilmicosin phosphate crystal. The method comprises the following steps of: firstly fully dissolving tilmicosin phosphate powder in ethyl acetate, then slowly dripping isopropyl ether under the temperature condition of 0-5 DEG C in a stirring state for mixing, keeping the stirring state for 30-60min after the end of dripping, and performing solid-liquid separation, leaching and vacuum drying. According to the preparation method disclosed by the invention, tilmicosin phosphate is prepared into crystal particles, and the crystal particles are used for replacing the powder; as the specific gravity of the crystal particles is lager, the dust pollution can be avoided during packaging and using processes; furthermore, drinking water for animals is added, the crystal particles are easy to settle down into the water bottom, the dispersion is better, the dissolution speed is higher, the content is higher, and the crystal particles can be directly added into animal feed or the drinking water for the animals; and in addition, a solvent is very easy to recover, and the tilmicosin phosphate crystal further has certain application prospects in production.

Description

technical field [0001] The invention belongs to the technical field of antibiotic products, in particular to a method for preparing tilmicosin phosphate crystals. Background technique [0002] Tilmicosin Phosphate is a semi-synthesized antibiotic for livestock and poultry from the hydrolyzate of tylosin. The drug was first successfully developed by the American Elanco Animal Health Products Company in the 1980s. At present, the Ministry of Agriculture of my country has approved some veterinary pharmaceutical factories to produce tilmicosin Coxin raw materials, premixes, solutions and injections. [0003] At present, in the production process of tilmicosin phosphate, spray drying is used to prepare its salt products. During the production and packaging process, a large amount of dust pollution is likely to be generated, causing certain injuries to the operator; during use, tilmicosin phosphate is added to feed or drinking water for animals, and due to the small specific grav...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/06
Inventor 王义任勇周丽娜
Owner 宁夏泰瑞制药股份有限公司
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