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Analytic method for related substance examination of rebamipide

A technology of rebamipide and mass analysis, applied in the direction of analyzing materials, material separation, measuring devices, etc., can solve unreliable problems

Active Publication Date: 2013-05-01
北京元延医药科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method was used to test, and the system suitability solution was used to verify the test. The results showed that the method could not effectively separate the 4 known impurities.
Therefore, the results determined by the above two chromatographic conditions are unreliable, thereby unable to carry out reliable and effective quality control of rebamipide

Method used

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  • Analytic method for related substance examination of rebamipide
  • Analytic method for related substance examination of rebamipide
  • Analytic method for related substance examination of rebamipide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] Instruments and conditions:

[0061] Shimadzu 2010AH all-in-one high-performance liquid chromatography and Shimadzu's LC-solution workstation; octadecylsilane-bonded silica gel as a filler column (Unilmate, XB-C18, 4.6mm×15cm×5μm, month Asahi); with methanol as mobile phase A, with phosphate buffer (take potassium dihydrogen phosphate 6.8g, add 0.1mol / L sodium hydroxide solution 152ml, add 10% tetrabutylammonium hydroxide solution 10ml, add water to 1000ml, use Phosphoric acid to adjust the pH to 6.5, shake well, to get) is mobile phase C, mobile phase is mobile phase A methanol and mobile phase C phosphate buffer according to the volume ratio of 45:55; detection wavelength is 235nm; column temperature is 35 ℃. Mobile phase flow rate: 1.0ml / min, liquid phase analysis injection volume: 20μl, automatic injection.

[0062] experiment procedure:

[0063] Weigh an appropriate amount of 4-(bromomethyl)-2-quinolinone, intermediate 1, intermediate 2, ortho-chloro isomer and ...

Embodiment 2

[0073] Instruments and conditions:

[0074] Shimadzu 2010AH all-in-one high-performance liquid chromatography and Shimadzu's LC-solution workstation; octadecylsilane-bonded silica gel as a filler column (Unilmate, XB-C18, 4.6mm×15cm×5μm, month Asahi); with methanol as mobile phase A, with phosphate buffer (get 6.8g of potassium dihydrogen phosphate, add 0.1mol / L sodium hydroxide solution 152ml, add 10% tetrabutylammonium hydroxide solution 10ml, add water to 1000ml, use Phosphoric acid to adjust the pH to 6.5, shake well, to get) is mobile phase C, mobile phase is mobile phase A methanol and mobile phase C phosphate buffer according to the volume ratio of 45:55; detection wavelength is 235nm; column temperature is 35 ℃. Mobile phase flow rate: 1.0ml / min, liquid phase analysis injection volume: 20μl, automatic injection.

[0075] experiment procedure:

[0076] Get rebamipide (crude drug) in an appropriate amount, dissolve with mobile phase, and be mixed with the need testing...

Embodiment 3

[0080] Instruments and conditions:

[0081] Shimadzu 2010AH all-in-one high-performance liquid chromatography and Shimadzu's LC-solution workstation; octadecylsilane-bonded silica gel as a filler column (Unilmate, XB-C18, 4.6mm×15cm×5μm, month Asahi); with methanol as mobile phase A, with phosphate buffer (get 6.8g of potassium dihydrogen phosphate, add 0.1mol / L sodium hydroxide solution 152ml, add 10% tetrabutylammonium hydroxide solution 10ml, add water to 1000ml, use Phosphoric acid to adjust the pH to 6.5, shake well, to get) is mobile phase C, mobile phase is mobile phase A methanol and mobile phase C phosphate buffer according to the volume ratio of 45:55; detection wavelength is 235nm; column temperature is 35 ℃. Mobile phase flow rate: 1.0ml / min, liquid phase analysis injection volume: 20μl, automatic injection.

[0082] experiment procedure:

[0083] Get the rebamipide tablet, dissolve it with the mobile phase, and be prepared into a test solution approximately equ...

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Abstract

The invention relates to an analytic method for related substance examination of rebamipide, in particular to a method for mass analysis of rebamipide. The method comprises the step of adopting the high-performance liquid chromatography to achieve mass analysis of rebamipide drug substances or pharmaceutical preparations containing rebamipide. A chromatographic column used in the method is a C18 chromatographic column with the column temperature of 30 DEG C-40 DEG C. The analytic method effectively separate rebamipide and all impurities of rebamipide under a certain chromatographic condition, and can accurately measure the quantities of all the impurities in rebamipide.

Description

technical field [0001] The invention belongs to the field of pharmaceutical analytical chemistry, and relates to a method for analyzing the quality of the antiulcer drug rebamipide, in particular to an analysis method for separating and measuring rebamipide and various known impurities thereof by liquid chromatography. Background technique [0002] Rebamipide (Rebamipide, CAS No:90098-04-7), the chemical name is (±)-2-(4-chlorobenzamido)-3-[2(1H)-quinolone-4]propionic acid , the molecular formula is C19H15ClN2O4, the molecular weight is 370.79, and its structural formula is as follows: [0003] [0004] Rebamipide is a drug for treating gastric ulcer. It was first launched in 1990 as a new type of anti-ulcer drug developed and produced by Otsuka Pharmaceutical Co., Ltd. of Japan. The starting material that is used to synthesize this product has 4-(bromomethyl)-2-quinolinone (abbreviated as impurity A in the present invention), can bring ortho-chloro isomer (referred to a...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 王立强张燕霞冯连松
Owner 北京元延医药科技股份有限公司
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