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A kind of refining method of tetracycline

A refining method and tetracycline technology, applied in organic chemistry, carboxylic acid amide separation/purification, etc., can solve the problems of cumbersome operation, low product yield and purity, etc., and achieve simple equipment, simple and feasible refining method, and high economic benefits Effect

Active Publication Date: 2016-04-27
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

[0004] The purpose of the present invention is to provide a method for refining tetracycline, which solves the problems of low product yield and purity and cumbersome operation in existing refining methods

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The refining method of the tetracycline of the present embodiment comprises the following steps:

[0026] 1) Take 10g of crude tetracycline and add it to hydrochloric acid with a pH of 1.0, stir to dissolve, then add ammonium thiocyanate and borax to dissolve to obtain mixture A, the mass concentration of ammonium thiocyanate in mixture A is 1.5%, and the mass concentration of borax 1.5%;

[0027] 2) Adjust the pH of the mixture A to 1.2 with hydrochloric acid, let it stand for 1 hour and then filter until clear to obtain the filtrate A;

[0028] 3) Add zinc sulfate, potassium ferrocyanide, and activated carbon to filtrate A, the mass ratio of zinc sulfate to potassium ferrocyanide is 0.5:1, heat and stir at 50°C for 30 minutes to obtain mixture B, zinc sulfate in mixture B The total mass concentration of potassium ferrocyanide and potassium ferrocyanide is 4.0g / L, the mass concentration of activated carbon is 4.0g / L, the mixture B is left to stand for 2h, and filtered...

Embodiment 2

[0033] The refining method of the tetracycline of the present embodiment comprises the following steps:

[0034] 1) Take 10g of crude tetracycline and add it to sulfuric acid with a pH of 1.0, stir to dissolve, then add ammonium thiocyanate and borax to dissolve to obtain mixture A, the mass concentration of ammonium thiocyanate in mixture A is 2.5%, and the mass concentration of borax 2.0%;

[0035] 2) Adjust the pH of the mixture A to 1.5 with hydrochloric acid, let it stand for 1 hour, and then filter until clear to obtain the filtrate A;

[0036] 3) Add zinc sulfate, potassium ferrocyanide, and activated carbon to filtrate A, the mass ratio of zinc sulfate to potassium ferrocyanide is 0.6:1, heat and stir at 55°C for 30 minutes to obtain mixture B, zinc sulfate in mixture B The total mass concentration of potassium ferrocyanide and potassium ferrocyanide is 6.0g / L, the mass concentration of activated carbon is 6.0g / L, the mixture B is left to stand for 2h, and filtered un...

Embodiment 3

[0041] The refining method of the tetracycline of the present embodiment comprises the following steps:

[0042] 1) Add 10 g of crude tetracycline into hydrochloric acid with a pH of 1.0, stir to dissolve, then add ammonium thiocyanate and borax to dissolve, and obtain mixture A. The mass concentration of ammonium thiocyanate in mixture A is 3.0%, and the mass concentration of borax 2.5%;

[0043] 2) Adjust the pH of the mixture A to 1.2 with hydrochloric acid, let it stand for 1 hour and then filter until clear to obtain the filtrate A;

[0044] 3) Add zinc sulfate, potassium ferrocyanide, and activated carbon to filtrate A, the mass ratio of zinc sulfate to potassium ferrocyanide is 0.8:1, heat and stir at 60°C for 30 minutes to obtain mixture B, zinc sulfate in mixture B The total mass concentration of potassium ferrocyanide and potassium ferrocyanide is 5.0g / L, the mass concentration of activated carbon is 9.0g / L, the mixture B is left to stand for 2h, and filtered until ...

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PUM

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Abstract

The invention discloses a refining method for tetracycline. The method comprises the following steps: (1) adding crude tetracycline into an acid solvent, and adding an acid precipitant and borax for dissolving to obtain a mixture A; (2) adjusting the pH of the mixture A to 1.2-2.8, standing the mixture A, and filtering the mixture A to obtain filtrate A; (3) adding zinc sulfate, potassium ferrocyanide and active carbon into the filtrate A to obtain a mixture B, standing the mixture B, and filtering the mixture B to obtain filtrate B; (4) performing ultrafiltration on the filtrate B to obtain filtrate C, adjusting the pH of the filtrate C to 4.5-5.0, standing the filtrate C, and filtering the filtrate C to obtain a filter cake A; (5) taking the filter cake A out, dissolving the filter cake A by using the acid solvent, adjusting the pH of the dissolved filter cake A to 4.5-5.0, standing the dissolved filter cake A, and filtering the dissolved filter cake A to obtain a filter cake B; and (6) drying the filter cake B in vacuum to obtain refined tetracycline. The refining method disclosed by the invention has the advantages of high product yield, high product purity, easiness and feasibility in operation, need of simple equipment, adoption of cheap and readily-available raw materials and low cost, and is suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of antibiotic purification, and in particular relates to a method for refining tetracycline. Background technique [0002] Tetracycline is a broad-spectrum tetracycline antibiotic, mainly used to prevent and treat rickettsia, mycoplasma, chlamydia and some Gram-negative bacteria infections in pigs, cattle, sheep and poultry, and for dysentery, skin suppurative infection and endemic pneumonia It has obvious curative effect. Tetracycline 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] Most of them are oral-grade crude tetracyclines in the market at present, and the number of times of medication is high, which causes strong animal stress reactions, and contains impurities such as pyrogens and viruses, which easily cause toxic reactions; High, and the operation is cumbersome, which is...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C237/26C07C231/24
Inventor 张听盼李亚娥李建正王沛
Owner 河南后羿制药有限公司
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