A kind of preparation method of tartaric acid/tylosin phosphate

A technology of tylosin phosphate and tylosin, which can be used in the preparation of sugar derivatives, chemical instruments and methods, organic chemistry, etc., and can solve the problems that impurities cannot be effectively separated.

Active Publication Date: 2021-04-20
QILU PHARMA INNER MONGOLIA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In the above extraction process, extraction is performed after filtration. During the extraction process of the filtrate after filtration, some proteins that have not been removed by filtration will enter the organic phase, and some fatty acids produced by fermentation will also enter the ester phase, resulting in impurities that cannot be effectively extracted. separate

Method used

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  • A kind of preparation method of tartaric acid/tylosin phosphate
  • A kind of preparation method of tartaric acid/tylosin phosphate
  • A kind of preparation method of tartaric acid/tylosin phosphate

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Embodiment 1

[0033] A preparation method of tartaric acid / tylosin phosphate, comprising steps as follows:

[0034] Tylosin fermentation broth volume 10m 3 , titer 12386U / mL, total billion is 123.9. Add polyaluminum chloride, the weight ratio of polyaluminum chloride to fermentation broth is 1.0±0.3% (w / w), and stir for 25±5 minutes. Filter the fermentation broth with a plate and frame filter, control the feed pressure to 0.3MPa, and obtain the filtrate after pressure filtration, which is the tylosin filtrate with a volume of 12m 3 , the titer is 9621U / mL.

[0035] The sodium hydroxide solution with a mass concentration of 3% and the filtrate are pumped into the mixer at the same time, the pH is controlled at 7.7, and the mixed feed liquid is injected into a centrifuge and centrifuged at a speed of 4500 rpm for 2 seconds to obtain purified After the filtrate; send the purified filtrate, butyl acetate and liquid caustic soda into the mixer to mix, adjust the pH value in the range of 9.8, ...

Embodiment 2

[0037] A preparation method of tartaric acid / tylosin phosphate, comprising steps as follows:

[0038] Tylosin fermentation broth volume 9.5m 3 , titer 13194U / mL, total billion is 126.9. A polyaluminum chloride solution with a mass concentration of 20-22% is added, the mass volume ratio of the polyaluminum chloride solution to the fermentation broth is 0.6% (w / v), and the mixture is stirred for 40 minutes. Filter the fermentation broth with a plate and frame filter, control the pressure of the filter press to 4.0MPa, and obtain the filtrate after the press filter, which is the tylosin filtrate with a volume of 11m 3 , the titer is 10832U / mL.

[0039] The sodium hydroxide solution with a mass concentration of 4wt% and the filtrate are pumped into the mixer at the same time, the pH is controlled at 7.9, and the mixed feed liquid is injected into the centrifuge and centrifuged at a speed of 4800 rpm for 2s to obtain Purified filtrate; send the purified filtrate, butyl acetate, ...

Embodiment 3

[0041] A kind of preparation method of tartaric acid / tylosin phosphate, described in embodiment 1, difference is:

[0042] The sodium hydroxide solution with a mass concentration of 3wt% and the filtrate are pumped into the mixer at the same time, the pH is controlled at 7.54, and the extraction is carried out after centrifugation.

[0043] pass figure 1 and figure 2 Contrast, it can be clearly seen that the impurity peaks in the chromatogram of the filtrate after purification are significantly less than figure 1 ,pass image 3 and Figure 4 Contrast, it can be clearly seen that the impurity peaks in the chromatogram of the filtrate after purification are significantly less than image 3 ,pass Figure 5 and Figure 6 Contrast, it can be clearly seen that the impurity peaks in the chromatogram of the filtrate after purification are significantly less than Figure 5 , Therefore, after the purification process of the present invention, it can be confirmed by HPLC that the...

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Abstract

The invention relates to a preparation method of tartaric acid / tylosin phosphate. The fermented liquid filtered by the present invention can separate the special protein that has not been filtered out in the fermented liquid through the specific lye and specific pH, and the fermented protein can be separated by centrifugation. The special protein that has not been filtered out in the liquid, the fatty acid produced by fermentation, and some oils are completely removed, and it has a purification effect on the solvent butyl acetate, which promotes the efficient extraction. While purifying the solvent, it will not cause any other effects on the solvent. Guarantee The extraction is carried out smoothly, and at the same time, the operation is simple and the cost is low. The simple and low-cost treatment method can achieve efficient and thorough reduction of impurities in the fermentation filtrate, and improve the purity and solubility of the product.

Description

technical field [0001] The invention relates to a preparation method of tartaric acid / tylosin phosphate, belonging to the technical field of biological pesticide preparation. Background technique [0002] Tylosin was first isolated from Thai soil by American scholar Hamill et al. The producing bacteria include Streptomyces freundii (S. .hygro-scopicus); Tylosin active ingredients include: Tylosin A (true tylosin), Tylosin B (decarbase sugar tylosin Desmycosin) and Tylosin C (big Mucrosin) and Tylosin D (Relomysin), component A≥80%, total component A+B+C+D≥95%, titer>800IU. The chemical structural formulas of the active ingredients of Tylosin are shown in Table 1 below: [0003] Table 1 [0004] [0005] The fermentation of tylosin uses soybean oil as the main carbon source. Glucose has obvious inhibitory effect on the biosynthesis of tylosin. If there is excessive glucose in the fermentation of differentiation stage, it will promote the increase of ATP level, there...

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 成祥兴范泽雷居亚东刘萍
Owner QILU PHARMA INNER MONGOLIA
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