Method for separating related substances of tulathromycin

A technology of telamycin and related substances, applied in the field of antibiotic separation and extraction, can solve the problems of low purity of target products, incomplete separation, incomplete reaction, etc., and achieve stable production batches, reliable quality, improved purity, and short production cycle Effect

Inactive Publication Date: 2019-03-12
JIANGSU WEI LING BIOCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The invention provides a method for separating related substances of telamycin, which solves the problems of low purity, incomplete separation and incomplete reaction of the separated target product proposed in the background technology

Method used

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  • Method for separating related substances of tulathromycin
  • Method for separating related substances of tulathromycin
  • Method for separating related substances of tulathromycin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 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.

[0035] 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

[0037] 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.

[0038] 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

[0040] 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, carry out isocratic elution, The ultraviolet absorption wavelength is 205nm, and the flow rate is 60ml / min.

[0041] 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 tel...

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Abstract

The invention provides a method for separating related substances of tulathromycin. High performance liquid chromatography is adopted, a to-be-separated object is washed in a chromatographic column through a flow phase, a qualified fraction is subjected to decompression distillation, and after extraction and desalting, an organic layer is taken to be subjected to decompression concentration to bedried. Before extraction, the qualified fraction is treated, the qualified fraction is subjected to high-pressure homogenization or ultrasonic crushing, the particle size is decreased, the pH is adjusted, activated carbon for an injection is added and stirred, decarbonization is conducted, then filtering is conducted through a filter membrane, thus the apparent distribution volume is increased, and impurities in the fraction are better separated out; and according to the separation method, the impurities generated in the synthesis and degradation processes of the tulathromycin can be effectively separated, the production batch is stable, the quality is reliable, the production period is short, the single-time preparation yield is high, the impurity weight control needs are met, and a goodfoundation is laid for the study of unknown impurities of the tulathromycin.

Description

technical field [0001] The invention belongs to the field of separation and extraction of antibiotics, and in particular relates to a separation method of related substances of telamycin. Background technique [0002] Tulathromycin is a semi-synthetic macrolide antibiotic that was launched in the US and EU 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 be strictly controlled. Drug con...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/00C07H1/06
CPCC07H1/06C07H17/00
Inventor 凌青云陈海刘言华杨玲卫
Owner JIANGSU WEI LING BIOCHEM TECH CO LTD
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