Method for detecting small polar impurities in pazufloxacin mesylate bulk drug

A technology for pazufloxacin mesylate and an API is applied in the field of quality control of the pazufloxacin mesylate API, which can solve problems such as ineffective detection and achieve the effect of scientific quality control

Inactive Publication Date: 2021-11-26
HAINAN HAISHEN TONGZHOU PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The inventor finds after studying a large amount of HPLC detection methods, the flow that these HPLC detection methods adopts is relative to the impurity of small polarity, especially the impurity that retention time is greater than main drug pazufloxacin mesylate characteristic peak, and cannot effectively detect

Method used

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  • Method for detecting small polar impurities in pazufloxacin mesylate bulk drug
  • Method for detecting small polar impurities in pazufloxacin mesylate bulk drug
  • Method for detecting small polar impurities in pazufloxacin mesylate bulk drug

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Embodiment 1 is used to detect the screening of the mobile phase of small polar impurity

[0036] The mobile phase pazufloxacin mesylate raw materials in Table 1 below were used for detection.

[0037] Table 1

[0038] mobile phase 1 Acetonitrile-10% triethylamine methanesulfonate-1M dipotassium hydrogen phosphate-water (30:10:7:170) mobile phase 2 Acetonitrile-10% triethylamine methanesulfonate-1M dipotassium hydrogen phosphate-water (30:10:7:153) mobile phase 3 Acetonitrile-10% triethylamine methanesulfonate-1M dipotassium hydrogen phosphate-water (45:10:7:138) mobile phase 4 Acetonitrile-10% triethylamine methanesulfonate-1M dipotassium hydrogen phosphate-water (70:10:7:113)

[0039] Wherein, the preparation of 10% triethylamine methanesulfonate solution is as follows:

[0040] Under the condition of ice bath, slowly add 30ml of methanesulfonic acid and 30ml of triethylamine into 200ml of water, after the dissolution is complete,...

Embodiment 2

[0052] Example 2 HPLC qualitative detection of Pazufloxacin mesylate bulk drug after photodegradation

[0053] Using mobile phase 3, other chromatographic conditions are the same as in Example 1.

[0054] The detection steps are as follows:

[0055] (1) Preparation of photodegradation test solution: take 30 mg of this product, put it in a 100 ml measuring bottle, use mobile phase to make a solution containing 300 μg of pazufloxacin mesylate per 1 ml, put it under ultraviolet light for 7 days, and use it as a Test solution.

[0056] (2) Perform HPLC detection according to the same method as in Example 1. Chromatograms such as figure 2 shown.

[0057] from figure 2 It can be seen from the figure that for the bulk drug after photodegradation, the small polar impurities produced by the degradation can be comprehensively and effectively removed by using the mobile phase provided by the application within the retention time of the characteristic peak of pazufloxacin mesylate ...

Embodiment 3

[0058] Example 3 The HPLC qualitative detection of the acid-degraded pazufloxacin mesylate crude drug uses mobile phase 3, and other chromatographic conditions are the same as in Example 1.

[0059] The detection steps are as follows:

[0060](1) Prepare the test solution for acid degradation: take 30 mg of pazufloxacin mesylate crude drug, put it in a 50 ml measuring bottle, add 25 ml of 1.0 mol / L hydrochloric acid and heat it in a boiling water bath for 12 hours in the dark, and add 1.0 mol / L sodium hydroxide was diluted and neutralized to the mark as the test solution.

[0061] (2) Perform HPLC detection according to the same method as in Example 1. Chromatograms such as image 3 shown. from image 3 It can be seen from the figure that for the bulk drug after acid degradation, the small polar impurities produced by the degradation can be comprehensively and effectively removed by using the mobile phase provided by the application within the retention time of the charact...

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Abstract

The invention discloses a method for detecting small polar impurities in pazufloxacin mesylate bulk drug, which adopts high performance liquid chromatography for detection, and the mobile phase is acetonitrile-10% triethylamine mesylate solution-1. 0mol / L dipotassium phosphate-water with the volume ratio of 45: 10: 7: 138; the method comprises the following steps: respectively taking a test solution and a contrast solution, injecting the test solution and the contrast solution into a high performance liquid chromatograph, and recording the retention time of a chromatogram to 7 times of a pazufloxacin mesylate characteristic peak. According to the present invention, the pazufloxacin mesylate bulk drug is detected by using the HPLC, and the small polar impurity with the retention time greater than the characteristic peak of the pazufloxacin mesylate can be effectively detected within the 7-time retention time of the pazufloxacin mesylate by using the specific ratio of the mobile phase; therefore, the quality control of the pazufloxacin mesilate bulk drug can be realized more accurately and scientifically.

Description

technical field [0001] The application relates to the field of quality control of the raw materials of pazufloxacin mesylate, in particular to a detection method for small polar impurities in the raw materials of pazufloxacin mesylate. 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] Pazufloxacin mesylate API may produce some degradation products after exposure to light, oxidation, high temperature, and acid and alkali during storage, transportation and use. These degradation products may affect the efficacy and even safety of the drug. wil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/34G01N30/86G01N30/74G01N30/88
CPCG01N30/02G01N30/34G01N30/8634G01N30/74G01N30/88G01N2030/8872Y02A50/30
Inventor 刘玉韦家华王汕桃
Owner HAINAN HAISHEN TONGZHOU PHARM CO LTD
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