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Method for preparing 4-epitetracycline from tetracycline urea double salt crystallization mother solution

A technology of epitetracycline and urea compound salt, which is applied in the fields of biology and medicine, can solve the problems such as the lack of 4-epicycline recovery, and achieves the effects of reducing content, reducing pressure, and achieving remarkable effects.

Active Publication Date: 2015-05-13
NINGXIA QIYUAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no recovery technology for 4-episocycline in tetracycline urea double salt crystallization mother liquor.

Method used

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  • Method for preparing 4-epitetracycline from tetracycline urea double salt crystallization mother solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Take 1L tetracycline urea double salt crystallization mother liquor, measure the potency unit of mother liquor 8057u / ml (wherein 4- epitetracycline potency unit 7110u / ml, 4-epiprine tetracycline potency unit 34u / ml, anhydrotetracycline potency unit 141u / ml), add 300g oxalic acid, adjust PH=2.2, control the temperature at 35°C, stir for 30 minutes, filter with double-layer 621 filter cloth, cool the filtrate temperature to 18°C, start to pass 13% ammonia water, 30 minutes evenly Add 70ml dropwise, adjust the pH to 5.0, continue to cool down to 9°C, stir and crystallize for 60 minutes, centrifuge, rinse with purified water, blow air into the air for dehydration, and obtain 10.1g of crude 4-epeptracycline with a water content of 27.5%. Add 1L of water to the crude 4-differential tetracycline, adjust the pH to 2.3 with reagent hydrochloric acid, stir to dissolve, add 13% ammonia water, add 62ml evenly within 30 minutes, adjust the pH to 5.4, control the temperature at 10°C, ...

Embodiment 2

[0017] Take 1L of tetracycline urea mother liquor, measure the potency unit of urea mother liquor 8104u / ml (among them, the potency unit of 4-episocycline is 7459u / ml, the potency unit of 4-epiprine tetracycline is 67u / ml, and the potency unit of anhydrotetracycline is 96u / ml ), add 280g oxalic acid, adjust PH=2.4, control the temperature at 33°C, stir for 30 minutes, then filter with double-layer 621 filter cloth, cool the filtrate temperature to 20°C, start to introduce 13% ammonia water, and add 58ml dropwise evenly in 30 minutes, Adjust the pH to 4.9, continue to lower the temperature to 12°C, stir and crystallize for 60 minutes, centrifuge, rinse with purified water, blow air into the air for dehydration, and obtain 9.95 g of crude 4-epipridine with a water content of 27.2%. Add 1L of water, adjust pH=2.3 with reagent hydrochloric acid, stir to dissolve, add 13% ammonia water, add 60ml evenly dropwise within 30 minutes, adjust pH=5.2, control temperature at 12°C, stir and ...

Embodiment 3

[0019] Take 1L of tetracycline urea mother liquor, measure the titer unit of urea mother liquor 7995u / ml (among them, the potency unit of 4-episocycline is 7853u / ml, the potency unit of 4-epiprine tetracycline is 47u / ml, and the potency unit of anhydrotetracycline is 78u / ml ), add 280g oxalic acid, adjust PH=2.3, control the temperature at 35°C, stir for 30 minutes, then filter with double-layer 621 filter cloth, cool the filtrate to 22°C, start to pass in 13% ammonia water, and add 69ml dropwise evenly in 30 minutes, Adjust the pH to 5.0, continue to cool down to 10°C, stir and crystallize for 60 minutes, centrifuge, rinse with purified water, blow air into the air for dehydration, and obtain 10.0 g of crude 4-apeptracycline with a water content of 27.0%. Add 1L of water, adjust pH=2.5 with reagent hydrochloric acid, stir to dissolve, add 13% ammonia water, add 61ml evenly dropwise within 30 minutes, adjust pH=5.3, control temperature at 10°C, stir and crystallize for 60 minut...

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Abstract

The invention relates to a method for preparing 4-epitetracycline from a tetracycline urea double salt crystallization mother solution. The method comprises the steps of firstly, acidifying the tetracycline urea double salt crystallization mother solution until the pH value is 1.0-3.0; then stirring for 10-40 minutes at 25-40 DEG C, then filtering by using double-layer 621 filter cloth, cooling the obtained filtrate to 18-22 DEG C, introducing ammonia water uniformly and slowly, controlling the temperature to be 5-20 DEG C when the pH value is 4.0-6.0, and stirring for 60-120 minutes to perform crystallization; finally, separating, leaching and dehydrating to obtain a 4-epitetracycline crude product, and controlling the water content to be less than or equal to 32%. The quality of 4-epitetracycline prepared by the method disclosed by the invention can meet a quality standard of a standard product of 4-epitetracycline, and 4-epitetracycline is used for inspecting and detecting content, impurities and the like, and removing and using tetracycline and isomeride in a urea mother solution at the same time, so that the content of antibiotics in the mother solution is greatly reduced to ensure that the tetracycline urea mother solution can be treated by using a biochemical method more easily, the pressure of environmental protection treatment is reduced, and the effect is significant.

Description

technical field [0001] The invention relates to the technical field of biology and medicine, in particular to a method for preparing 4-epimetridine from tetracycline urea double salt crystallization mother liquor. Background technique [0002] The mother liquor produced during the production process of tetracycline urea double salt crystallization contains 5000u / ml~16000u / ml of tetracycline and isomers of tetracycline such as 4-epitetracycline, anhydrotetracycline, 4-epipetracycline and isotetracycline, Most of them are 4-epimine. Due to the bacteriostatic properties of residual tetracycline and its isomers, it is difficult to deal with the mother liquor biochemical method, and the pressure on environmental protection is very high, so it is impossible to achieve clean production. Therefore, it is necessary to recycle the tetracycline urea double salt crystallization mother liquor. In the prior art, the method for recovering the tetracycline urea double salt crystallization...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C237/26C07C231/24
Inventor 沈卫军李学兵王良郭海燕邹学锋张志
Owner NINGXIA QIYUAN PHARMA