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Method for separating and purifying tulathromycin D

A telamycin, separation and purification technology, applied in the field of separation and purification of telamycin D, can solve the problems of incomplete separation, low purity of the target product, incomplete reaction, etc., to achieve improved purity and stable quality of production batches Reliable, short lead time results

Pending Publication Date: 2020-12-15
JIANGSU WEI LING BIOCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The invention provides a method for separation and purification of Tyramycin D, which solves the problems of low purity, incomplete separation, and incomplete reaction of the isolated target product proposed in the background technology, so that Tyramycin can be better separated Elemental impurity D, improve the purity of telamycin

Method used

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  • Method for separating and purifying tulathromycin D
  • Method for separating and purifying tulathromycin D
  • Method for separating and purifying tulathromycin D

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Chromatographic parameters: C18, 5um filler packing 250g, mobile phase A is 0.01mol / L trisodium phosphate aqueous solution, mobile phase B is acetonitrile and methanol, trisodium phosphate aqueous solution: mobile phase B=40:60, for isocratic elution, The ultraviolet absorption wavelength is 205nm, and the flow rate is 60ml / min.

[0053] The specific process steps are as follows: first dissolve the to-be-separated material, then soak the ion exchange fiber as the separation material in the solution, let it stand for 50 minutes, and then filter out the solution; heat the ammonia water to 65°C, soak the above The ion-exchange fiber that has adsorbed telamycin and telamycin-related substances for 160 minutes was filtered off ammonia; butyl formate was added in an amount 3 times that of the ion-exchange fiber to obtain the pretreated analyte, That is, the treated crude telamycin. Use 10mL of acetonitrile to dissolve 2g of crude telamycin in a neutral environment, filter th...

Embodiment 2

[0055] Chromatographic parameters: C18, 10um filler packing 250g, mobile phase A is 0.01mol / L potassium dihydrogen phosphate aqueous solution, mobile phase B is acetonitrile and ethanol, potassium dihydrogen phosphate solution: mobile phase B=15:85, carry out isocratic washing Desorption, ultraviolet absorption wavelength 205nm, flow rate 60ml / min.

[0056] The specific process steps are as follows: first dissolve the to-be-separated material, then soak the ion-exchange fiber as the separation material in the solution, let it stand for 60 minutes, and then filter out the solution; heat the ammonia water to 61°C, soak the above The ion-exchange fiber that has adsorbed telamycin and telamycin-related substances for 100 minutes was filtered off ammonia; butyl formate was added in an amount 2.5 times that of the ion-exchange fiber to obtain the pretreated analyte, That is, the treated crude telamycin. Use 150mL of acetonitrile to dissolve 1g of crude telamycin in a neutral enviro...

Embodiment 3

[0058] Chromatographic parameters: C8, 10um filler packing 250g, mobile phase A is 0.01mol / L potassium dihydrogen phosphate aqueous solution, mobile phase B is acetonitrile, potassium dihydrogen phosphate aqueous solution: mobile phase B=25:75, for isocratic elution, The ultraviolet absorption wavelength is 205nm, and the flow rate is 60ml / min.

[0059] The specific process steps are as follows: firstly dissolve the material to be separated, then soak the ion exchange fiber as the separation material in the solution, let it stand for 70 minutes, and then filter out the solution; heat the ammonia water to 60°C, take the ammonia water and soak the above The ion-exchange fiber that has adsorbed telamycin and telamycin-related substances for 80 minutes was filtered off ammonia; butyl formate was added in an amount twice that of the ion-exchange fiber to obtain the pretreated analyte, That is, the treated crude telamycin. Use 5 mL of acetonitrile to dissolve 1 g of crude telamycin...

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Abstract

The invention provides a method for separating and purifying tulathromycin D. The method comprises the following steps: eluting a to-be-separated substance in a chromatographic column by using a mobile phase by adopting high performance liquid chromatography, performing reduced pressure distillation on qualified fractions, extracting and desalting, and performing reduced pressure concentration onan organic layer until the organic layer is dried. According to the method disclosed by the invention, the qualified fractions are treated before extraction, the qualified fractions are subjected to high-pressure homogenization or ultrasonic grinding, the particle size is reduced, the pH value is regulated, activated carbon for injection is added, stirring and decarburization are performed, filtration is performed by virtue of a filter membrane, the apparent distribution volume is improved, and impurities in the fractions are well separated. According to the separation method, the impurities produced in the synthesis and degradation process of the tulathromycin can be effectively separated, the production batch is stable, the quality is reliable, the production cycle is short, the single preparation yield is high, the impurity quality control requirements are met, and a good foundation is laid for research of unknown impurities of the tulathromycin.

Description

technical field [0001] The invention belongs to the field of separation and extraction of antibiotics, in particular to a method for separation and purification of telamycin D. Background technique [0002] Tulathromycin (Tulathromycin) is a semi-synthetic macrolide antibiotic that was launched in the United States and the European Union in 2004. The drug is mainly used for the prevention and treatment of respiratory infectious diseases caused by sensitive bacteria in cattle and pigs and infectious keratoconjunctivitis caused by Moraxella bovis. Rhythromycin and tilmicosin have broad prospects for use in livestock and poultry production. [0003] Tyramycin is a 15-membered ring macrolide antibiotic composed of isomers A and B (molecular formula C41H79N3O12, molecular weight 806.09) at a ratio of 9:1. The formation and breaking of ester bonds carry out transformations. [0004] In order to ensure the safety of animal-derived food, the quality of animal-specific drugs must ...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/00C07H1/06
CPCC07H17/08C07H1/00C07H1/06
Inventor 凌青云陈海刘言华杨玲卫
Owner JIANGSU WEI LING BIOCHEM TECH CO LTD
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