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Tulathromycin related substance, enriching and preparation method and application thereof

A technology of telamycin and related substances, applied in the field of telamycin-related substances, can solve the problems of lack of telamycin separation, detection methods, inability to identify and confirm the structure, etc.

Active Publication Date: 2016-11-23
SHANGHAI INST OF PHARMA IND +1
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  • 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

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  • Tulathromycin related substance, enriching and preparation method and application thereof
  • Tulathromycin related substance, enriching and preparation method and application thereof
  • Tulathromycin related substance, enriching and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0094] 5mg tyramycin bulk drug was dissolved in 1mL 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 adjusted to pH 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 the MS detection with a 3:1 split. The total ion current of the mass spectrometer is as figure 1 As shown, the impurities are shown in Table 1. When the mobile phase salt concentration is 0.35%, the main peak retention time is appropriate and the peak shape is 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 teramycin and its impuriti...

Embodiment 2

[0105] 5mg tyramycin crude drug was dissolved in 1mL 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 adjusted to pH 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 the MS detection with a 3:1 split. The total ion current of the mass spectrometer is as Image 6 Shown. When the mobile phase salt concentration is 0.3%, the main peak retention time is appropriate and the peak shape is good. Related substances can be well separated from the main peak.

Embodiment 3

[0108] 5mg tyramycin crude drug was dissolved in 1mL 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 to adjust the pH value of 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 the MS detection with a 3:1 split. The total ion current of the mass spectrometer is as Figure 7 Shown. When the mobile phase salt concentration is 0.4%, the main peak retention time is appropriate and the peak shape is good. Related substances can be well separated from the main peak.

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Abstract

The invention discloses a telamycin related substance, its enrichment preparation method and application. The present invention provides a telamycin related substance 3 or a salt thereof. The present invention also provides a method for enriching telamycin-related substances 3, which includes the following steps: using high-performance liquid chromatography to elute the analyte in a chromatographic column, and collecting telamycin-related substances 3 is enough. The telamycin-related substance of the present invention is a necessity for quality control of the telamycin; the enrichment preparation method of the present invention can effectively separate the telamycin-related substance 3, thereby controlling the drug quality of the telamycin, for The study of unknown impurities of telamycin has laid a good foundation.

Description

Technical field [0001] The invention relates to a tyramycin related substance, its enriched preparation method and application. Background technique [0002] Tulathromycin (Tulathromycin) is a semi-synthetic macrolide antibiotic, which was marketed in the United States and the European Union in 2004. The drug is mainly used for the prevention and treatment of infectious diseases of the respiratory system caused by sensitive bacteria in cattle and pigs and the prevention and treatment of infectious keratoconjunctivitis caused by Moraxella bovis. Its efficacy is stronger than that of macrolide antibiotics widely used in the market. Tylosin and Tilmicosin have broad application prospects in livestock and poultry production. [0003] Teramycin is composed of isomers A and B (molecular formula C 41 H 79 N 3 O 12 , Molecular weight 806.09) is a 15-membered ring macrolide antibiotic composed of 9:1. The two isomers can be converted by the formation and cleavage of the lactone bond betwee...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 李悦黄珊
Owner SHANGHAI INST OF PHARMA IND
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