Method for detecting 9-nitrominocycline in tigecycline for injection

A technology of nitrominocycline and tigecycline, which is applied in the detection field of 9-nitrominocycline in tigecycline for injection, and can solve the problem that 9-nitrominocycline cannot be quantified effectively And other issues

Active Publication Date: 2020-04-24
瀚晖制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The main purpose of the present invention is to provide a detection method for 9-nitrominocycline in tigecycline for injection, to solve the problem of trace 9-nitrominocycline in tigecycline for injection in the prior art. Cyclocycline can not be effectively quantified problem

Method used

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  • Method for detecting 9-nitrominocycline in tigecycline for injection
  • Method for detecting 9-nitrominocycline in tigecycline for injection
  • Method for detecting 9-nitrominocycline in tigecycline for injection

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The process of establishing the standard curve

[0042] The standard solution preparation process is as follows:

[0043] The standard solution is the system suitability solution: use methanol to dilute 14.1 mg of 9-nitrominocycline standard sample (equivalent to 12 mg of 9-nitrominocycline) step by step, and prepare them respectively to a concentration of 0.05 μg / mL , a single standard solution of 0.25 μg / mL carries out the detection process of high performance liquid chromatography tandem mass spectrometry to the standard solution as follows:

[0044] The conditions for HPLC detection are set as follows: the chromatographic column is a Welch XB-C18 chromatographic column, and the chromatographic column size is 4.6×50mm, 5μm, the column temperature is 35°C, the flow rate is 0.5ml / min, and the mobile phase A is volume The formic acid content is 0.1%, the mobile phase B is acetonitrile, and the gradient elution process is: 0 ~ 2min using 75% mobile phase A and 25% mob...

Embodiment 2

[0071] Different from the detection conditions of Example 1, the details are as follows.

[0072] The conditions for HPLC detection are set as follows: the chromatographic column is a Welch XB-C18 chromatographic column, and the chromatographic column size is 4.6×50mm, 5μm, the column temperature is 30°C, the flow rate is 0.3ml / min, and the mobile phase A is volume The formic acid content is 0.2%, the mobile phase B is acetonitrile, and the gradient elution process is: 0 ~ 2min using 70% mobile phase A and 30% mobile phase B for elution, 2 ~ 8min using 1% mobile phase A and 99% mobile phase B was used for elution, and 70% mobile phase A and 30% mobile phase B were used for elution in 8-13 minutes.

[0073] The conditions for mass spectrometry detection are set as follows: the ion source is AJS ESI, the drying gas temperature is 310°C, the drying gas flow rate is 9L / min, the atomizing gas pressure is 30psi, the sheath gas temperature is 330°C, and the sheath flow rate is 10L / mi...

Embodiment 3

[0076] Different from the detection conditions of Example 1, the details are as follows.

[0077] The conditions for HPLC detection are set as follows: the chromatographic column is a Welch XB-C18 chromatographic column, and the chromatographic column size is 4.6×50mm, 5μm, the column temperature is 40°C, the flow rate is 0.8ml / min, and the mobile phase A is volume The content is 0.05% formic acid, mobile phase B is acetonitrile, the gradient elution process is: 0 ~ 2min adopts 80% mobile phase A and 20% mobile phase B to elute, 2 ~ 8min adopts 3% mobile phase A and 97% mobile phase B was used for elution, and 80% mobile phase A and 20% mobile phase B were used for elution in 8-13 minutes.

[0078] The conditions for mass spectrometry detection are set as follows: the ion source is AJS ESI, the drying gas temperature is 280°C, the drying gas flow rate is 7L / min, the atomizing gas pressure is 40psi, the sheath flow gas temperature is 360°C, and the sheath flow flow rate is 12L / ...

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Abstract

The invention provides a method for detecting 9-nitrominocycline in tigecycline for injection. The detection method comprises the following steps: step S1, obtaining a standard curve of high performance liquid chromatography tandem mass spectrometry of 9-nitrominocycline, wherein the vertical coordinate of the standard curve is the characteristic ion peak area of 9-nitrominocycline, and the horizontal coordinate is the mass content of 9-nitrominocycline; step S2, dissolving tigecycline for injection to form a tigecycline solution, and performing high performance liquid chromatography tandem mass spectrometry detection on the tigecycline solution to obtain a mass chromatogram; and step S3, determining the characteristic ion peak of the 9-nitrominocycline in the mass chromatogram according to the analysis result of the mass chromatogram, and calculating the mass content of the 9-nitrominocycline by taking the peak area of the characteristic ion peak as the basis of the standard curve. According to the detection method, the accurate mass content of the 9-nitrominocycline can be obtained and a reliable data basis can be provided for effective mass control of the 9-nitrominocycline.

Description

technical field [0001] The invention relates to the technical field of quality control of tigecycline, in particular to a method for detecting 9-nitrominocycline in tigecycline for injection. Background technique [0002] Tigecycline (Tigecycline), developed by the Wyeth Pharmaceutical Company of the United States, is a new type of broad-spectrum active intravenous antibiotics. It is also active against drug-resistant methicillin-resistant Staphylococcus aureus. It is a glycylcycline class The first drug in , has the following chemical structure: [0003] [0004] According to the synthesis process of tigecycline, known impurities that may exist in tigecycline include epiminocycline, minocycline, 9-aminominocycline, 9-nitrominocycline, N - tert-butylglycine, epimers, oxides, quinone analogs, tricyclics, etc., among which 9-nitrominocycline is a key intermediate for the production of tigecycline, and is a genotoxic Impurities. However, in the prior art, the quantitative...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/027G01N2030/8872
Inventor 徐慧娟杜加秋姜丽丽赵技宇夏莉
Owner 瀚晖制药有限公司
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