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Novel preparation method for florfenicol crystal

A florfenicol, a new type of technology, applied in the field of new preparation of florfenicol crystals, can solve problems such as difficult large-scale application, inconvenient application of injections, unreliable safety, etc., to achieve enhanced collision and ultra- Miniaturization effect, excellent effect

Active Publication Date: 2019-04-02
京山瑞生制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And injection is difficult to be applied on a large scale in large-scale farms due to inconvenient application.
Moreover, most of the injections are prepared with organic solvents such as dimethylformamide and propylene glycol, which are likely to cause local irritation and toxicity, and are unreliable in safety.
[0006] At present, the preparation of florfenicol superfine powder has become the development trend of the industry, but florfenicol products are easy to crystallize, and it is very difficult to obtain superfine powder products
The ultrafine pulverization equipment common in the industry is not only inefficient, but also the particle size of the obtained micropowder is generally larger than 20 microns

Method used

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  • Novel preparation method for florfenicol crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) In the reaction kettle 2, add solvent tetrahydrofuran, dissolve the former powder of florfenicol in tetrahydrofuran, and prepare a tetrahydrofuran solution of florfenicol, wherein the concentration of florfenicol is 30mg / ml.

[0029] (2) In another reaction kettle 2, an anti-solvent aqueous solution is prepared, which contains ethanol at a concentration of 5% and sodium hyaluronate at a concentration of 0.5%.

[0030] (3) The anti-solvent aqueous solution in step 2 is started with strong stirring, controlled at a temperature of -20 ° C, and the tetrahydrofuran solution of florfenicol is quickly pumped into the liquid surface of the anti-solvent aqueous solution through the high-pressure delivery pump 3. The opposite jet outlet 1 and the flow velocity at the outlet pipe is greater than 3 m / s. Continue vigorous stirring for 60 min. A suspension of florfenicol was obtained. Wherein the volume ratio of the anti-solvent aqueous solution to the tetrahydrofuran solution ...

Embodiment 2

[0033] (1) In the reaction kettle 2, add solvent tetrahydrofuran, dissolve the former powder of florfenicol in tetrahydrofuran, and prepare a tetrahydrofuran solution of florfenicol, wherein the concentration of florfenicol is 80mg / ml.

[0034] (2) In another reaction kettle 2, prepare an aqueous anti-solvent solution, which contains ethanol at a concentration of 1%; contains sodium hyaluronate 0.1%.

[0035] (3) Turn on the strong stirring of the anti-solvent aqueous solution in step 2, and control the temperature at 0°C, and quickly pump the tetrahydrofuran solution of florfenicol into the liquid surface of the anti-solvent aqueous solution through the high-pressure delivery pump 3. Type jet outlet 1 and the flow velocity at the outlet pipe is greater than 3 m / s. Continue vigorous stirring for 30 min. A suspension of florfenicol was obtained. Wherein the volume ratio of the anti-solvent aqueous solution to the tetrahydrofuran solution of Florfenicol is 50:1.

[0036] (4) ...

Embodiment 3

[0038] (1) In reaction kettle 2, add solvent tetrahydrofuran, dissolve the former powder of florfenicol in tetrahydrofuran, prepare the tetrahydrofuran solution of florfenicol, wherein the concentration of florfenicol is 50mg / ml.

[0039] (2) In another reaction kettle 2, an anti-solvent aqueous solution is prepared, which contains ethanol at a concentration of 3%; contains sodium hyaluronate 0.3%.

[0040] (3) The anti-solvent aqueous solution in step 2 is started to stir vigorously, controlled at a temperature of -10°C, and the tetrahydrofuran solution of florfenicol is quickly pumped under the liquid surface of the anti-solvent aqueous solution through the high-pressure delivery pump 3. The opposite jet outlet 1 and the flow velocity at the outlet pipe is greater than 3 m / s. Continue vigorous stirring for 60 min. A suspension of florfenicol was obtained. Wherein the volume ratio of the anti-solvent aqueous solution to the tetrahydrofuran solution of Florfenicol is 25:1. ...

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Abstract

The invention discloses a novel preparation method for a florfenicol crystal, comprising the steps of adding a solvent tetrahydrofuran in a reaction kettle, dissolving a florfenicol raw powder in thetetrahydrofuran to prepare a tetrahydrofuran solution with a concentration of 30 mg / ml-80 mg / ml; preparing an anti-solvent water solution in another reaction kettle, and the like. The method of the invention adopts an anti-solvent method for recrystallization to obtain a florfenicol ultrafine powder, and has two major advantages: one advantages is that an aqueous solution containing sodium hyaluronate / ethanol is employed and has extremely excellent ultra-micronization effect, and the other advantage is that an opposite jetting outlet is employed for strengthening the collision between droplets, is beneficial to breakage of the droplets and is beneficial for achieving of the ultra-micronization effect.

Description

technical field [0001] The invention belongs to the technical field of organic chemistry, and in particular relates to a novel preparation method for preparing florfenicol crystals. Background technique [0002] Florfenicol (Florfenicol) Chinese name: fluprofen; [0003] Compared with similar chloramphenicol and thiamphenicol, florfenicol has the characteristics of broad antibacterial spectrum, good absorption, wide distribution in the body, safety and high efficiency, and has no potential aplastic anemia, teratogenicity, carcinogenicity and Mutagenicity, especially chloramphenicol is prohibited from being used in food animals due to severe aplastic anemia adverse reactions. Therefore, florfenicol has broad application prospects in the prevention and treatment of food animal diseases. However, Florfenicol is insoluble in water, and the solubility in water is only 1350 μg / ml, which not only affects the oral absorption of Florfenicol, but also further affects its bioavailabil...

Claims

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Application Information

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IPC IPC(8): C07C315/06C07C317/32
CPCC07C315/06C07C317/32
Inventor 张治国徐相雨钟旭辉周国朝
Owner 京山瑞生制药有限公司
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