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Method for refining oxytetracycline

A refining method and technology of oxytetracycline, applied in organic chemistry, carboxylic acid amide separation/purification, etc., can solve the problems of unfavorable wide application, cumbersome operation, low purity of oxytetracycline, etc., achieve no toxic side effects, cheap and easy raw materials Obtaining and refining methods are simple and feasible

Active Publication Date: 2014-07-30
河南后羿制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the purity of oxytetracycline produced by the current method for refining oxytetracycline is not high, and the operation is cumbersome, which is not conducive to the wide application in industry

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The refining method of the oxytetracycline provided by the present embodiment, the concrete steps are as follows:

[0021] 1) Take 10g of crude oxytetracycline and dissolve it in hydrochloric acid with pH=1.0;

[0022] 2) Add 1.5g / ml ammonium thiocyanate to the above solution to dissolve, add hydrochloric acid to adjust the pH to 1.2, let stand for 1h, filter until clear, and take the filtrate;

[0023] 3) Add 4.0g / ml zinc sulfate and potassium ferrocyanide to the above filtrate, the mass ratio is 0.5:1, stir, let stand for 2h, filter until clear, and take the filtrate;

[0024] 4) The above filtrate is subjected to ultrafiltration at 0.10Mpa, and the molecular weight cut-off of the ultrafiltration membrane is 10K;

[0025] 5) Take the above ultrafiltrate, adjust its pH to 4.5 with potassium hydroxide solution, let it stand for 4 hours, filter it with medium-speed filter paper, and take the filter cake;

[0026] 6) Dissolve the above filter cake with hydrochloric acid...

Embodiment 2

[0033] The refining method of the oxytetracycline provided by the present embodiment, the concrete steps are as follows:

[0034] 1) Take 10g of crude oxytetracycline and dissolve it in hydrochloric acid with pH=1.0;

[0035] 2) Add 2.5g / ml ammonium thiocyanate to the above solution to dissolve, then add hydrochloric acid to adjust the pH to 1.5, let it stand for 1h, filter, and take the filtrate;

[0036] 3) Add 6.0g / ml zinc sulfate and potassium ferrocyanide to the above filtrate, the mass ratio is 0.6:1, stir, let stand for 2h, filter until clear, and take the filtrate;

[0037] 4) The above filtrate is subjected to ultrafiltration at 0.10Mpa, and the molecular weight cut-off of the ultrafiltration membrane is 20K;

[0038] 5) Take the above ultrafiltrate, adjust its pH to 4.8 with sodium hydroxide solution, let it stand for 4 hours, filter it with medium-speed filter paper, and take the filter cake;

[0039] 6) Dissolve the above filter cake with hydrochloric acid with p...

Embodiment 3

[0046] The refining method of the oxytetracycline provided by the present embodiment, the concrete steps are as follows:

[0047] 1) Take 10g of crude oxytetracycline and dissolve it in hydrochloric acid solution with pH=1.0;

[0048] 2) Add 3.0g / ml ammonium thiocyanate to the above solution to dissolve, then adjust the pH to 1.8 with hydrochloric acid, let it stand for 1h, filter, and take the filtrate;

[0049] 3) Add 5.0g / ml zinc sulfate and potassium ferrocyanide to the above filtrate, the mass ratio is 0.8:1, stir, let stand for 2h, filter until clear, and take the filtrate;

[0050] 4) The above filtrate is subjected to ultrafiltration at 0.10Mpa, and the molecular weight cut-off of the ultrafiltration membrane is 30K;

[0051] 5) Take the above ultrafiltrate, adjust its pH to 5.0 with ammonia water, let it stand for 4 hours, filter, and take the filter cake;

[0052] 6) Dissolve the above filter cake with hydrochloric acid solution with pH=1.0, then adjust the pH to 5...

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PUM

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Abstract

The invention discloses a method for refining oxytetracycline. The method particularly comprises the following steps: 1) dissolving coarse oxytetracycline into hydrochloric acid; 2) adding ammonium thiocyanate, dissolving with stirring, adjusting the pH value of the solution, standing for 1 hour and then filtering impurities; 3) adding potassium hexacyanoferrate-zinc sulfate scavenging agent into the filtrate, standing for 2 hours and then filtering impurities; 4) performing ultrafiltration on the filtrate; 5) adjusting the pH value of the ultrafiltrate to be 4.5-5.0, standing for 4 hours and then filtering to obtain crystal; 6) dissolving the crystal with hydrochloric acid adjusting the pH value to be 4.5-5.0, standing for 4 hours and then filtering to obtain crystal; and 7) carrying out vacuum-drying on the crystal to obtain the refined oxytetracycline. The method for refining the oxytetracycline is simple and low in cost. The prepared oxytetracycline has high purity, stable physiological and biochemical characteristics, no toxic or side effect and wide application value.

Description

technical field [0001] The invention relates to a method for refining oxytetracycline, belonging to the field of antibiotic preparations. Background technique [0002] Oxytetracycline is a broad-spectrum tetracycline antibiotic, mainly used for the prevention and treatment of Rickettsia, Mycoplasma, Chlamydia and some Gram-negative bacteria infections in pigs, cattle, sheep and poultry, for dysentery, skin suppurative infection and local pneumonia has obvious curative effect. Oxytetracycline is slightly soluble in water, soluble in organic solvents such as ethanol, and can be made into powder, injection, etc., which is convenient for clinical application. [0003] Oral-grade crude oxytetracycline, which is administered frequently, causes strong stress reactions in animals, and contains impurities such as pyrogens and viruses, which can easily cause toxic reactions. The refined oxytetracycline has high drug efficacy and less impurities, thereby greatly reducing the stress r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C237/26C07C231/24
Inventor 吴红云李建正张听盼
Owner 河南后羿制药有限公司
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