A related substance of telamycin, its enrichment preparation method and application

A technology of tebramycin and related substances, applied in the field of tebramycin related substances, can solve the problems of lack of separation and detection methods of tebramycin, inability to identify, confirm the structure and the like

Active Publication Date: 2019-01-01
SHANGHAI INST OF PHARMA IND CO LTD +1
View PDF7 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The problem to be solved by the present invention is to overcome the lack of methods for the separation and detection of related substances produced during the synthesis and degradation of telamycin in the prior art, and the inability to identify and confirm the structure and other defects, and provide a A telamycin related substance, its enrichment preparation method and application

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A related substance of telamycin, its enrichment preparation method and application
  • A related substance of telamycin, its enrichment preparation method and application
  • A related substance of telamycin, its enrichment preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0094] 5mg of telamycin API was dissolved in 1mL of acetonitrile, and the injection volume was 20μL.

[0095] Chromatographic parameters: Xbridge TM C 18 (250*4.6mm, 5μm) column, mobile phase A: 0.35% formic acid aqueous solution (ammonia water to adjust the pH value to 7.66), mobile phase B: methanol:acetonitrile=45:25, gradient elution 0→15min, A:B=65 :35; 15→40min, A:B=65:35→30:70; 40→55min, A:B=30:70, UV absorption wavelength 205nm, column temperature 35℃, flow rate 1.0ml / min, HPLC fraction After passing through the UV detector, it enters MS detection with a 3:1 split. mass spectrometric total ion current as figure 1 Shown, each impurity is as shown in table 1. When the salt concentration of the mobile phase was 0.35%, the retention time of the main peak was appropriate and the peak shape was good. Related substances can be well separated from the main peak. It can be seen from the figure that the method of the present invention can be used to detect telamycin and i...

Embodiment 2

[0105] 5mg of telamycin API was dissolved in 1mL of acetonitrile, and the injection volume was 20μL.

[0106] Chromatographic parameters: Xbridge TM C 18 (250*4.6mm, 5μm) column, mobile phase A: 0.3% formic acid aqueous solution (ammonia water to adjust the pH value to 7.66), mobile phase B: methanol:acetonitrile=45:25, gradient elution 0→15min, A:B=65 :35; 15→40min, A:B=65:35→30:70; 40→55min, A:B=30:70, UV absorption wavelength 205nm, column temperature 35℃, flow rate 1.0ml / min, HPLC fraction After passing through the UV detector, it enters MS detection with a 3:1 split. mass spectrometric total ion current as Figure 6 shown. When the salt concentration of the mobile phase was 0.3%, the retention time of the main peak was appropriate and the peak shape was good. Related substances can be well separated from the main peak.

Embodiment 3

[0108] 5mg of telamycin API was dissolved in 1mL of acetonitrile, and the injection volume was 20μL.

[0109] Chromatographic parameters: Xbridge TM C 18 (250*4.6mm, 5μm) column, mobile phase A: 0.4% formic acid aqueous solution (ammonia water adjusts the pH value to 7.66), mobile phase B: methanol:acetonitrile=45:25, gradient elution 0→15min, A:B=65 :35; 15→40min, A:B=65:35→30:70; 40→55min, A:B=30:70, UV absorption wavelength 205nm, column temperature 35℃, flow rate 1.0ml / min, HPLC fraction After passing through the UV detector, it enters MS detection with a 3:1 split. mass spectrometric total ion current as Figure 7 shown. When the salt concentration of the mobile phase was 0.4%, the retention time of the main peak was appropriate and the peak shape was good. Related substances can be well separated from the main peak.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
concentrationaaaaaaaaaa
absorption wavelengthaaaaaaaaaa
Login to view more

Abstract

The invention discloses a tulathromycin related substance, an enriching and preparation method and an application thereof. The invention provides a tulathromycin related substance (3) or a salt thereof and also provides the enriching and preparation method of the tulathromycin related substance (3). The method includes the steps of: through high performance liquid chromatography, eluting a to-be-tested substance in a chromatographic column, and collecting the tulathromycin related substance (3). The tulathromycin related substance is a necessary substance of quality control of tulathromycin. The method can effectively separate the tulathromycin related substance (3) so as to control the quality of the tulathromycin, thus laying an excellent fundament for researching on unknown impurities of the tulathromycin.

Description

technical field [0001] The invention relates to a telamycin related substance, its enrichment preparation method and application. 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 bovine infectious keratoconjunctivitis caused by Moraxella bovis, and its efficacy is stronger than that of macrolide antibiotics widely used in the market Tylosin and tilmicosin have broad prospects for use in livestock and poultry production. [0003] Tyramycin is composed of isomers A and B (molecular formula C 41 h 79 N 3 o 12 , molecular weight 806.09) is a fifteen-membered ring macrolide antibiotic composed of 9:1, and the two isomers can be converted through the formation and cleavage of the lactone bond between C11 and C13. Tyramycin contains three polar amino group...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 李悦黄珊
Owner SHANGHAI INST OF PHARMA IND CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap