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Acetylisovaleryltylosin tartrate purifying method

A technology of tivalamectin and purification method, which is applied in the field of antibiotic purification, can solve the problem of low product purity, and achieve the effect of overcoming the low product purity

Active Publication Date: 2015-05-13
CHINA ANIMAL HUSBANDRY IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to solve the above-mentioned technical problems, an object of the present invention is to provide a new method for purifying tivalamectin by silica gel chromatography, so as to overcome the problem that the purity of the product obtained by the existing tivalamectin purification process is too low

Method used

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  • Acetylisovaleryltylosin tartrate purifying method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Dissolve 100 g of crude tivalamectin (purity about 75%) obtained by fermentation with an appropriate amount of ethyl acetate, add 400 g of 100-200 mesh column chromatography silica gel, mix well, spin evaporate to dryness, and apply the sample by dry method. When loading the sample, the column chromatography silica gel mixed with tivalamectin was placed in a glass column pre-filled with 2 kg pre-packed column chromatography silica gel, and the packed silica gel chromatography column was rinsed with petroleum ether.

[0056] Utilize ethyl acetate and petroleum ether to prepare the mixed solution with the volume ratio shown in Table 4, and add diethylamine with a volume ratio of 0.1% to the mixed solution, carry out gradient elution as the eluent, and use high performance liquid chromatography The eluate was monitored for tivalancin.

[0057] Table 4 gradient elution method

[0058] eluent volume ratio

[0059] The collected eluted fractions containing high-pur...

Embodiment 2

[0061] Dissolve 400 g of crude tivalamectin (purity about 75%) obtained by fermentation with an appropriate amount of ethyl acetate, add 400 g of 200-300 mesh column chromatography silica gel, mix well, spin evaporate to dryness, and apply the sample by dry method. When loading the sample, the column chromatography silica gel mixed with tivalamectin was placed in a glass column pre-filled with 4 kg pre-packed column chromatography silica gel, and the packed silica gel chromatography column was rinsed with petroleum ether.

[0062] Utilize ethyl acetate and sherwood oil to prepare mixed solution with the volume ratio shown in Table 5, and add volume ratio in mixed solution and be 0.05% triethylamine, carry out gradient elution as eluent, and utilize high performance liquid chromatography The eluate was monitored for tyvalancin.

[0063] Table 5 gradient elution method

[0064] eluent volume ratio

[0065] The collected eluted fractions containing high-purity tivalanc...

Embodiment 3

[0067] Dissolve 200 g of crude tivalamectin (purity about 75%) obtained by fermentation with an appropriate amount of butyl acetate, add 400 g of 100-200 mesh silica gel for column chromatography, mix well, spin evaporate to dryness, and apply the sample by dry method. When loading the sample, the column chromatography silica gel mixed with tivalamectin is placed in a glass column pre-filled with 2.8kg pre-packed column chromatography silica gel, and the packed silica gel chromatography column is rinsed with petroleum ether .

[0068] Use butyl acetate and petroleum ether to prepare a mixed solution in the volume ratio shown in Table 6, and add 0.01% N,N-diisopropylethylamine in the mixed solution as the eluent for gradient elution , and use high performance liquid chromatography to monitor the eluent for tivalamectin.

[0069] Table 6 gradient elution method

[0070] eluent volume ratio

[0071] The collected eluted fractions containing high-purity tivalancin were...

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Abstract

The invention provides a novel method of utilizing silica gel chromatography to purify acetylisovaleryltylosin tartrate. The method comprises the following steps: using column-layer chromatographic silica gel as a separation medium; using mixed liquor comprising the following substances as an eluent to purify an acetylisovaleryltylosin tartrate crude product: 1) petroleum ether, 2) ethyl acetate and / or butyl acetate, and 3) one or more of diethylamine, triethylamine and N,N-diisopropylethylamine; further performing rotary evaporation to obtain high-purity acetylisovaleryltylosin tartrate. The method disclosed by the invention can effectively remove impurities, overcomes the problem that the product purity obtained according to the conventional acetylisovaleryltylosin tartrate purifying process is too low; the product purity of the acetylisovaleryltylosin tartrate prepared according to the method provided by the invention is up to 97% above.

Description

technical field [0001] The invention belongs to the field of antibiotic purification, and mainly relates to the purification technology of the antibiotic tivalamectin. Background technique [0002] Tyvanectin, also known as super tylosin, chemically named 3-O-acetyl-4”-O-isovaleryl tylosin, is a special antibiotic for livestock and poultry, and its structural formula is as follows. Tyvanectin is Tylosin is a new type of macrolide antibiotic obtained by biotransformation of Streptomyces thermotolerans, acetylation at the 3-position and isovalerylation at the 4” position. Compared with tylosin, it has obvious advantages in terms of antibacterial activity, drug resistance, chemical stability, oral absorption and blood drug concentration. [0003] [0004] Tyvalancin Chemical Structural Formula [0005] Chinese patent CN101381756A discloses a method for purifying super tylosin (i.e., tyvanectin) by using the method of acid extraction, alkali precipitation and secondary crys...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/06
CPCC07H1/06C07H17/08
Inventor 张国栋吴家鑫张传良徐金雷张刚王大旭齐鹏郑应华赵梅仙葛辛玫马佳颖宋敏张淼
Owner CHINA ANIMAL HUSBANDRY IND