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A kind of method for recrystallization of tylosin tartrate

A technology of tylosin tartrate and recrystallization, applied in chemical instruments and methods, organic chemistry, sugar derivatives, etc., can solve the problem of high price of extraction solvent butyl acetate, difficulty in final product components, general solubility and other problems, to achieve the effect of high content of tylosin A component, low cost and high product yield

Active Publication Date: 2021-03-19
NINGXIA TAIYICIN BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The extraction solvent butyl acetate used in this process has a high price, general solubility, strong volatility, and high toxicity; in addition, this process directly sprays and dries the refined solution to obtain the finished product of tylosin tartrate. Although the operation is simple and the production cycle is short, but If the B, C, and D components in the fermentation broth are too high, the process cannot effectively remove impurities, and it is difficult to make the final product components qualified

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Extraction: take 5m of the refined solution of tylosin tartrate 3 , the potency is 167840, and the total billion is 839.2kg. Use 1.0m 3 Extract with dichloromethane, the extraction ratio is tylosin tartrate refined solution: dichloromethane=5:1 (v:v), the extraction time is 0.5h, the extraction temperature is 30°C, and the raffinate titer is 357U / ml .

[0013] Recrystallization: Separate the phases of the above extract, discard the water phase, cool the dichloromethane phase to room temperature, then slowly add sec-butyl acetate dropwise to make tylosin tartrate reach supersaturation and crystallize. The dosage of sec-butyl acetate is 5.0m 3 . After the crystals were centrifuged and dried, 819.9 kg of the product was obtained, the yield was 97.7%, and the content of tylosin A was 94.2%.

Embodiment 2

[0015] Extraction: take 5m of the refined solution of tylosin tartrate 3 , the potency is 177521, and the total billion is 887.6kg. Use 1.3m 3 Extract with dichloromethane, the extraction ratio is tylosin tartrate refined solution: dichloromethane=4:1 (v:v), the extraction time is 1.0h, the extraction temperature is 40°C, and the raffinate titer is 123U / ml .

[0016] Recrystallization: Separate the phases of the above extract, discard the water phase, cool the dichloromethane phase to room temperature, then slowly add sec-butyl acetate dropwise to make tylosin tartrate reach supersaturation and crystallize. The dosage of sec-butyl acetate is 7.1m 3 . After the crystals were centrifuged and dried, 865.4 kg of the product was obtained, and the yield was 97.5%. The content of Tylosin A is 94.4%.

Embodiment 3

[0018] Extraction: take 5m of the refined solution of tylosin tartrate 3 , the potency is 180840, and the total billion is 904.2kg. Use 1.7m 3 Dichloromethane for extraction, the extraction ratio is tylosin tartrate refined liquid: dichloromethane=3:1 (v:v), the extraction time is 2.0h, the extraction temperature is 50°C, and the raffinate titer is 399U / ml .

[0019] Recrystallization: Separate the phases of the above extract, discard the water phase, cool the dichloromethane phase to room temperature, then slowly add sec-butyl acetate dropwise to make tylosin tartrate reach supersaturation and crystallize. The dosage of sec-butyl acetate is 8.1m 3 . Crystals were centrifuged and dried to obtain 887.9 kg of product, with a yield of 98.2%. The content of Tylosin A is 95.1%.

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Abstract

The invention relates to a method for recrystallizing tylosin tartrate. The method comprises the following process steps: firstly extracting a tylosin tartrate refined solution by using dichloromethane, slowly and dropwise adding sec-butyl acetate in a dichloromethane phase obtained after phase splitting until separating out crystal; then centrifuging and drying the crystal. According to the characteristic that the tylosin tartrate can be dissolved in the dichloromethane but not be dissolved in the sec-butyl acetate, the tylosin tartrate refined solution is subjected to recrystallization treatment by adopting a dichloromethane extracting and sec-butyl acetate crystallization separation method; the yield of a product obtained through the method disclosed by the invention is up to 97.0 percent or more, and the content of a tylosin component A is up to 94.0 percent or more; the method has the characteristics that technological treatment is simple, no pollution is generated, the cost is low, the period is short, the yield of the obtained product is high, the content of the tylosin component A is high, the quality is high, and the like.

Description

technical field [0001] The invention belongs to the technical field of antibiotic refining, in particular to a method for recrystallizing tylosin tartrate. Background technique [0002] Tylosin tartrate is the tartrate salt of tylosin. It is a special macrolide antibiotic for animals. It has a strong killing effect on pathogenic microorganisms such as Gram-positive bacteria and some Gram-negative bacteria. Under alkaline conditions, tylosin exists in the form of alkali and is easily soluble in organic solvents; under acidic conditions, it can combine with acids to form salts and is easily soluble in water. Taking advantage of this characteristic, the current preparation process of tylosin tartrate is to pretreat the tylosin fermentation liquid, filter with plate and frame, extract with butyl acetate, and back-extract with tartaric acid to obtain the water extract, then pass the water extract through medium and decolorization to obtain the refined solution of tylosin tartrat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/08C07H1/06
CPCC07H1/06C07H17/08
Inventor 梁丽娟王勇平陆建中郭佳张磊
Owner NINGXIA TAIYICIN BIOTECH CO LTD
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