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A kind of teramycin related substance, enrichment preparation method, separation method and application

A technology of tabramycin and separation method, which is applied in the preparation of sugar derivatives, material separation, chemical instruments and methods, etc., can solve the problems of inability to identify, confirm the structure, lack of separation and detection methods of tabramycin, etc.

Active Publication Date: 2019-04-12
SHANGHAI INST OF PHARMA IND CO LTD +1
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  • 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 separation and detection methods for related substances produced in the synthesis and degradation process of telamycin in the prior art, and the inability to identify and confirm the structure and other defects, and provide a Related substances of telamycin, enrichment preparation method, separation method and application

Method used

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  • A kind of teramycin related substance, enrichment preparation method, separation method and application
  • A kind of teramycin related substance, enrichment preparation method, separation method and application
  • A kind of teramycin related substance, enrichment preparation method, separation method and application

Examples

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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 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 Image 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.

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Abstract

The invention discloses a tulathromycin related substance, and an enriching preparing method, a separation method and an application thereof. The invention provides the separation method of the tulathromycin related substance, wherein the separation method comprises the following steps: adopting high performance liquid chromatography, eluting a to-be-tested material in a chromatographic column, and thus obtaining the product. The invention also provides the tulathromycin related substance 1 or a salt thereof. The separation method can effectively separate impurities produced in synthesis and degradation processes of tulathromycin, trace impurities can be detected further by mass spectrometric detection with high sensitivity, and the structure is identified and confirmed, so that the drug quality of tulathromycin is controlled, and a good foundation is laid for study of tulathromycin unknown impurities; the tulathromycin related substance is a necessity for quality control of tulathromycin.

Description

technical field [0001] The invention relates to a telamycin-related substance, a preparation method for enrichment, a separation 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 ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/00C07H1/06G01N30/06
Inventor 李悦黄珊
Owner SHANGHAI INST OF PHARMA IND CO LTD
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