Method for detecting related substances in pazufloxacin mesylate bulk drug by adopting HPLC

A technology of pazufloxacin mesylate and related substances, which is applied in the field of quality control of pazufloxacin mesylate, can solve problems such as unsatisfactory separation and ineffective detection of related substances, and achieve a suitable retention time Effect

Inactive Publication Date: 2021-11-09
HAINAN HAISHEN TONGZHOU PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The inventors of the present application have found that when the mobile phase is used for detection, the separation of related substances and the main drug (pazufloxacin mesylate) is not ideal
Moreover, the inventors further found that when the mobile phase is used to detect related substances, the relatively less polar related substances whose retention time is behind the main drug cannot be effectively detected.

Method used

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  • Method for detecting related substances in pazufloxacin mesylate bulk drug by adopting HPLC
  • Method for detecting related substances in pazufloxacin mesylate bulk drug by adopting HPLC
  • Method for detecting related substances in pazufloxacin mesylate bulk drug by adopting HPLC

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Embodiment 1 uses the first mobile phase Pazufloxacin mesylate crude drug to detect

[0041] The chromatographic conditions are as follows:

[0042] Stationary phase: Octadecylsilane bonded silica gel,

[0043] The first mobile phase: acetonitrile-10% triethylamine methanesulfonate-1M dipotassium hydrogen phosphate-water (30:10:7:170)

[0044] Flow rate: 1.0ml / min,

[0045] Detection wavelength: 254nm,

[0046] Injection volume: 20 μl.

[0047] The detection steps are as follows:

[0048] (1) Take 30mg of pazufloxacin mesylate crude drug, accurately weighed, put in a 100ml measuring bottle, add the first mobile phase to dissolve and dilute to the mark, shake well, and use it as the test solution.

[0049] (2) Under the condition of the first mobile phase, get need testing solution 20 μ l and inject the liquid chromatograph, record the chromatogram to 2 times of the retention time of the characteristic peak of pazufloxacin mesylate, the HPLC chromatogram is as follo...

Embodiment 2

[0057] Embodiment 2 uses the second mobile phase Pazufloxacin mesylate bulk drug to detect

[0058] The chromatographic conditions are as follows:

[0059] Stationary phase: Octadecylsilane bonded silica gel,

[0060]The second mobile phase: acetonitrile-10% triethylamine methanesulfonate-1M dipotassium hydrogen phosphate-water (45:10:7:138)

[0061] Flow rate: 1.0ml / min,

[0062] Detection wavelength: 254nm,

[0063] Injection volume: 20 μl.

[0064] The detection steps are as follows:

[0065] (1) Prepare the test solution according to the step (1) of Example 1.

[0066] (2) Under the condition of the second mobile phase, get need testing solution 20 μ l and inject the liquid chromatograph, record the chromatogram to 7 times of the retention time of the characteristic peak of pazufloxacin mesylate, the HPLC chromatogram is as follows Figure 2A shown.

[0067] From Figure 2A It can be seen that, for some related substances with less polarity and peaks after the rete...

Embodiment 3

[0073] Embodiment 3 jointly adopts the first mobile phase and the second mobile phase to detect pazufloxacin mesylate

[0074] The Pazufloxacin Mesylate API (internal batch number 0125) synthesized in-house was tested for related substances.

[0075] The detection steps are as follows:

[0076] (1) Get 30 mg of pazufloxacin mesylate crude drug, accurately weighed, put in a 100ml measuring bottle, add the first mobile phase to dissolve and dilute to the scale, shake up, as the test solution; Put 1ml of product solution in a 100ml measuring bottle, dilute to the mark with the first mobile phase, shake well, and use it as a control solution.

[0077] (2) Under the condition of the first mobile phase, get need testing solution and contrast solution and inject high-performance liquid chromatograph respectively, record chromatogram to 2 times of pazufloxacin mesylate characteristic peak retention time, need testing The chromatograms of the solution and the control solution are as ...

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Abstract

The invention discloses a method for detecting related substances in pazufloxacin mesylate by adopting HPLC, which comprises the following steps: preparing a test solution of a pazufloxacin mesylate bulk drug, and diluting the test solution to obtain a contrast solution; and according to the method, detecting a pazufloxacin mesylate bulk drug by taking acetonitrile-10% triethylamine mesylate solution and 1.0 mol / L dipotassium phosphate-water in a volume ratio of 30: 10: 7:170 as a first mobile phase and taking acetonitrile-10% triethylamine mesylate solution and 1.0 mol / L dipotassium phosphate-water in a volume ratio of 45:10:7:138 as a second mobile phase. Therefore, the first mobile phase and the second mobile phase are combined for use, so that the related substances of the pazufloxacin mesilate bulk drug can be detected more accurately and scientifically.

Description

technical field [0001] The invention relates to the field of quality control of pazufloxacin mesilate, in particular to a method for detecting related substances in a raw material drug of pazufloxacin mesilate by using HPLC. Background technique [0002] Pazufloxacin mesylate is a new type of fluoroquinolone antibacterial drug developed by Japan. It is the mesylate salt of Pazufloxacin. It has the characteristics of broad antibacterial spectrum, high antibacterial activity, small side effects and good tolerance. It is clinically used to treat Gram-positive and negative bacterial infections, such as bronchial and lung infections, bacillary dysentery, urinary system, skin and soft tissue infections. [0003] During the synthesis process of pazufloxacin mesylate and subsequent storage, transportation and use, some related substances (related substances) similar in structure to pazufloxacin mesylate may be produced. Efficacy and even safety may have an impact, therefore, for th...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/34G01N30/86G01N30/74
CPCG01N30/02G01N30/34G01N30/8634G01N30/74
Inventor 刘玉王汕桃
Owner HAINAN HAISHEN TONGZHOU PHARM CO LTD
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