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Method for detecting related substances of netilmicin sulfate injection

A technology for netilmicin sulfate and related substances, which is applied to measurement devices, instruments, scientific instruments, etc., can solve the problems of time-consuming and laborious, small space for optimization of chromatographic conditions, and low sensitivity.

Inactive Publication Date: 2018-07-24
江苏省食品药品监督检验研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Netilmicin retains a double bond in sisomicin structurally, and has weak ultraviolet absorption in the low wavelength region. In the current United States Pharmacopoeia, high performance liquid phase ultraviolet detector (HPLC-UV) is used to directly detect related substances. , but the main degraded impurity 1-N-ethylgalosamine with low sensitivity and no UV absorption cannot be detected
Numerous literature reports have used fluorescence or ultraviolet detection after pre-column or post-column derivatization with dansyl chloride and o-phthalaldehyde (OPA), which is low in sensitivity, time-consuming and laborious, with many factors affecting the experiment and poor reproducibility of results
The 2015 edition of "Chinese Pharmacopoeia" (ChP.2015) uses ELSD to detect its related substances, but there are problems such as low sensitivity, poor separation ability, and small space for optimization of chromatographic conditions.
The EP9.0 loaded PED method has high sensitivity, but the mobile phase contains a lot of salt, the column balance is difficult, the service life is short, and the separation is poor

Method used

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  • Method for detecting related substances of netilmicin sulfate injection
  • Method for detecting related substances of netilmicin sulfate injection
  • Method for detecting related substances of netilmicin sulfate injection

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Experimental program
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Effect test

Embodiment 1

[0047] Using the PED method of the present invention and the ChP.2015ELSD method, a total of 32 batches of netilmicin sulfate injection from 10 manufacturers were tested for related substances.

[0048] ChP.2015 ELSD method conditions

[0049] Mobile phase: 0.2M trifluoroacetic acid solution-methanol (84:16);

[0050] Flow rate: 0.5ml / min;

[0051] Chromatographic column: C18 (pH range 0.8 ~ 8.0);

[0052] Detector: evaporative light scattering detector;

[0053] Drift tube temperature: 100°C;

[0054] Carrier gas flow rate: 2.6L / min;

[0055] Concentration of the test product: 2mg / ml;

[0056] Injection volume: 20ul

[0057] Quantitative method: Take an appropriate amount of the test solution, and quantitatively dilute it with water to form a solution containing approximately 25 μg, 50 μg, and 100 μg of netilmicin per 1 ml, as a control solution, and use the logarithm value of the concentration of the control solution and the logarithm value of the peak area Calculate ...

Embodiment 2

[0063] 32 batches of netilmicin sulfate injection were checked for related substances by the PED method of the present invention, and the results obtained by the PED method were compared with the results by the ELSD method, and it was found that the number of impurities detected by the PED method and the amount of total impurities all increased significantly. Summarizing the PED impurity profile, it is found that 8 impurities appear most frequently, and their content is generally above 0.1%. Therefore, these 8 impurities are regarded as typical impurities in netilmicin sulfate injection. Currently known 1-N- Ethylgalosamine (No. 2 impurity) and sisomicin (No. 4 impurity) are two impurities, and the remaining 6 impurities are obtained by searching relevant literature and manual preparation after the column, and the corresponding fragment information is obtained through mass spectrometry. Based on this, it is inferred that The structure of each impurity is as follows:

[0064] N...

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Abstract

The invention provides a method for detecting related substances of a netilmicin sulfate injection. The method uses two ions to carry out gradient elution on a solution, a pulsed amperometric electrochemical detector is used for detecting, most of large-polarity impurities and a small part of impurities with higher polarity can be both taken into account, and the method has stronger separation ability, higher sensitivity, wider linear range, better specificity and excellent repeatability.

Description

technical field [0001] The invention relates to the field of drug analysis, and specifically provides a pulsed amperometric electrochemical detection method (PED) suitable for the detection of related substances in netilmicin sulfate injection. Background technique [0002] Netilmicin is a class of semi-synthetic aminoglycoside antibiotics, structural analysis is sisomicin 1-N-ethyl derivatives, also known as ethyl sisomicin. Netilmicin has a broad antibacterial spectrum and has strong antibacterial activity against Gram-negative bacteria and some Gram-positive bacteria. Netilmicin still has antibacterial activity against bacteria resistant to gentamicin, sisomicin, and tobramycin, and its ear and kidney toxicity is lower than that of the above aminoglycoside antibiotics, and its clinical application is its sulfate. [0003] Netilmicin retains a double bond in sisomicin structurally, and has weak ultraviolet absorption in the low wavelength region. In the current United Sta...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/64
CPCG01N30/06G01N30/64
Inventor 袁耀佐陈达赵卫张朝凤赵述强史孙亮张玫樊夏雷
Owner 江苏省食品药品监督检验研究院
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