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Preparation method of tylosin phosphate or tartrate crystal

A technology of tylosin tartrate and phosphate crystals, which is applied in the preparation of sugar derivatives, chemical instruments and methods, organic chemistry, etc. Slow dissolution and other problems, to achieve the effect of reducing physical harm, reducing pollution, and good dispersibility

Inactive 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, which causes great harm to the operator's body
When adding tylosin powder to feed or drinking water for animals, due to the small specific gravity of the powder, it floats on the water surface, which makes the dissolution of tylosin slow and affects normal use.
Some companies sell tylosin phosphate or tylosin tartrate as premixes or granules, but the content of tylosin 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

[0019] The preparation method of tylosin tartrate crystal:

[0020] (1) Dissolve tylosin tartrate powder in ethyl acetate solvent at a W:V ratio of 1:5 (unit: kg / L), mix and dissolve thoroughly.

[0021] (2) After complete dissolution, cool down to 0°C. When the temperature is stable, slowly add butyl acetate dropwise while stirring. The amount of butyl acetate added is 1 times the volume of ethyl acetate. At this time, a large amount of crystals are slowly precipitated. Add dropwise Stirring was maintained for 1 hour after completion.

[0022] (3) Centrifuge and wash the obtained crystals twice with cold butyl acetate 0.5 times the volume of ethyl acetate, and the temperature of cold butyl acetate is 0-2°C.

[0023] (4) At 60°C, use a double-cone rotary vacuum dryer to dry, and the vacuum degree is controlled at -0.08 to -0.02MPa, until the drying weight loss is less than 1%, and the crystal of tylosin tartrate is obtained, with a yield of 95%.

[0024] (5) Under the condit...

Embodiment 2

[0026] The preparation method of tylosin tartrate crystal:

[0027] (1) Dissolve tylosin tartrate powder in ethyl acetate solvent at a W:V ratio of 1:4 (unit: kg / L), and mix and dissolve thoroughly.

[0028] (2) After complete dissolution, cool down to 2°C. When the temperature is stable, slowly add butyl acetate dropwise while stirring. The amount of butyl acetate added is 1.5 times the volume of ethyl acetate. At this time, a large amount of crystals are slowly precipitated. Add dropwise Stirring was maintained for 1.5 hours after completion.

[0029] (3) After centrifugation, the obtained crystals were rinsed three times with 1-fold volume of ethyl acetate and butyl acetate. The temperature of cold butyl acetate is 0-2°C.

[0030] (4) Vacuum drying at 50°C until the loss on drying is less than 1%, to obtain tylosin tartrate crystals with a yield of 98%.

[0031] The solvent recovery is the same as in Example 1.

Embodiment 3

[0033] The preparation method of tylosin tartrate crystal:

[0034] (1) Dissolve tylosin tartrate powder in ethyl acetate solvent at a W:V ratio of 1:3 (unit: kg / L), mix and dissolve thoroughly.

[0035] (2) After complete dissolution, cool down to 5°C. When the temperature is stable, slowly add butyl acetate dropwise while stirring. The amount of butyl acetate added is twice the volume of ethyl acetate. At this time, a large amount of crystals are slowly precipitated. Add dropwise Stirring was maintained for 1 hour after completion.

[0036] (3) After centrifugation, the obtained crystals were rinsed twice with 1-fold volume of ethyl acetate and butyl acetate. The temperature of cold butyl acetate is 0-2°C.

[0037] (4) Vacuum drying at 60°C until the loss on drying is less than 1% to obtain tylosin tartrate crystals with a yield of 93%.

[0038] The solvent recovery is the same as in Example 1.

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PUM

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Abstract

The invention relates to a preparation method of tylosin phosphate or a tartrate crystal. The method comprises the steps that tylosin tartrate or phosphate powder is sufficiently dissolved in ethyl acetate; butyl acetate is slowly and dropwise added in a stirring state and at 0-5 DEG C, and is sufficiently mixed; the stirring state is kept for 1-2h after the adding is completed; centrifugal separation is performed; and the obtained crystal is subjected to drip washing by cold butyl acetate, and then subjected to vacuum drying until the drying loss is less than 1%. According to the preparation method, tylosin phosphate or tartrate is prepared into crystalline particles, and the crystalline particles replace powder; the specific gravity of the crystalline particles is greater, so that dust pollution is avoided in packaging and using processes; the particles are added to animal drinking water and can sink into the water bottom easily; the particles are better in dispersity, faster in dissolution rate and higher in content, can be directly added to animal feed or the animal drinking water; a solvent is very easy to recover; and the preparation method has a certain application prospect in a production process.

Description

technical field [0001] The invention belongs to the technical field of antibiotic product preparation, in particular to a method for preparing tylosin phosphate or tartrate crystals. Background technique [0002] Tylosin is a veterinary antibiotic produced by fermentation of Streptomyces freundii. At present, both at home and abroad, the fermentation broth is filtered, then extracted with an organic solvent, decolorized with activated carbon after stripping, concentrated, and spray-dried to obtain tylosin phosphate or tartrate. [0003] Currently, tylosin phosphate powder or tartrate powder is prepared by spray drying in the production of tylosin. The powder produces a large amount of dust during the packaging process, which causes great harm to the operator's body. When adding tylosin powder to feed or drinking water for animals, the powder has a small specific gravity and floats on the water surface, making the dissolution of tylosin slow and affecting normal use. Some ...

Claims

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Application Information

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