Method for separating and analyzing alogliptin benzoate and its related substance

A technology for separation and analysis of related substances, applied in the field of chemical analysis, can solve the problems of poor reproducibility of impurities, inaccurate integration, influence on the correct evaluation of preparation substances, etc., and achieve the effect of good elution separation effect and reliable separation effect.

Active Publication Date: 2016-04-27
WATERSTONE PHARMA WUHAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Patent CN103156819A in the prior art proposes to measure related substances with reference to the detection method of alogliptin benzoate raw material. However, the members of this research group found in the quality detection of finished products that an unknown impurity often appeared after the main peak of alogliptin. The unknown impurity was not found in the raw material testing and method verification, but in the precision test of the methodological research on the related substances of the preparation, it was found tha

Method used

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  • Method for separating and analyzing alogliptin benzoate and its related substance
  • Method for separating and analyzing alogliptin benzoate and its related substance
  • Method for separating and analyzing alogliptin benzoate and its related substance

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Experimental program
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Effect test

Embodiment 1

[0043] Instrument: Agilent1260 high performance liquid chromatography, DAD detector

[0044] Chromatographic column: Octyl bonded silica gel as filler (4.6mm×250mm, 5μm)

[0045] Mobile phase A: 0.04mol / L potassium dihydrogen phosphate buffer (containing 0.3% by volume of triethylamine), adjust pH to 3.0.0 with phosphoric acid

[0046] Mobile Phase B: Acetonitrile

[0047] See the table below for gradient elution:

[0048]

[0049] Flow rate: 1.0mL / min

[0050] Wavelength: 278nm

[0051] Column temperature: 30°C

[0052] Injection volume: 10μL

[0053] Diluent: mobile phase A

[0054] Experimental procedure: Take 20 tablets of the test product, weigh them accurately, calculate the average tablet weight, and grind them finely. Precisely weigh 30 mg fine powder equivalent to alogliptin into a 100 mL volumetric bottle, add 6 mL of 30% hydrogen peroxide solution to wet the sample for oxidative degradation, leave it at room temperature for 6 hours, add diluent to ultrason...

Embodiment 2

[0058] Instrument: Agilent1260 high performance liquid chromatography, DAD detector

[0059] Chromatographic column: Octyl bonded silica gel as filler (4.6mm×250mm, 5μm)

[0060] Mobile phase A: 0.04mol / L sodium dihydrogen phosphate buffer solution (containing 0.3% by volume of triethylamine), adjust the pH to 3.0 with phosphoric acid

[0061] Mobile Phase B: Acetonitrile

[0062] See the table below for gradient elution:

[0063]

[0064] Flow rate: 1.0mL / min

[0065] Wavelength: 278nm

[0066] Column temperature: 30°C

[0067] Injection volume: 10μL

[0068] Diluent: mobile phase A

[0069] Experimental procedure: Take 20 tablets of the test product, weigh them accurately, calculate the average tablet weight, and grind them finely. Precisely weigh approximately 30 mg of alogliptin fine powder into a 100 mL volumetric bottle, add 6 mL of 30% hydrogen peroxide solution to wet the sample for oxidative degradation, leave it at room temperature for 6 hours, add buffer s...

Embodiment 3

[0072] Instrument: Agilent1260 high performance liquid chromatography, DAD detector

[0073] Chromatographic column: Octyl bonded silica gel as filler (4.6mm×250mm, 5μm)

[0074] Mobile phase A: 0.04mol / L potassium dihydrogen phosphate buffer solution (containing 0.3% by volume of triethylamine), adjust the pH to 3.0 with phosphoric acid

[0075] Mobile Phase B: Acetonitrile

[0076] See the table below for gradient elution:

[0077]

[0078] Flow rate: 1.0mL / min

[0079] Wavelength: 278nm

[0080] Column temperature: 30°C

[0081] Injection volume: 10μL

[0082] Diluent: mobile phase A

[0083] Experimental procedure: Take 20 tablets of the test product, weigh them accurately, calculate the average tablet weight, and grind them finely. Precisely weigh approximately 30 mg of alogliptin fine powder into a 100 mL volumetric bottle, add 6 mL of 30% hydrogen peroxide solution to wet the sample for oxidative degradation, leave it at room temperature for 6 hours, add buffe...

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Abstract

The invention provides a method for separating and analyzing alogliptin benzoate and its related substance. The method takes octyl bonded silica gel as a fixed phase and takes a mixed solvent of a mobile-phase A-buffer, a mobile-phase B-organic solvent as a mobile phase for gradient elution. The method can rapidly and efficiently separate alogliptin benzoate and its related substance under same chromatographic condition, and the detection method has the advantages of strong specialization, high precision, strong accuracy and convenient operation, and can effectively control the medicine quality.

Description

technical field [0001] The invention relates to the field of chemical analysis, in particular to a method for separating and analyzing alogliptin benzoate preparations and related substances. Background technique [0002] Alogliptin benzoate (Alogliptinbenzoate, the structure shown in formula 1) is a DPP-IV inhibitor originally developed by Takeda Company in Japan, which can significantly inhibit DPP-IV with high selectivity and maintain GLP-1 and glucose levels in the body. It depends on the level of insulin-promoting polypeptide (GIP), promotes the secretion of insulin, and thus exerts the hypoglycemic effect. In April 2010, alogliptin benzoate was approved for marketing by the Ministry of Health, Labor and Welfare of Japan. Alogliptin benzoate (NESINA) of the original research manufacturer is a film-coated tablet, and there are 3 preparation specifications, with different specifications and different colors (25mg Yellow; 12.5mg slightly yellow; 6.25mg light red). The co...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/34
Inventor 祝小芬钱丽娜王珍刘大鹏崔健
Owner WATERSTONE PHARMA WUHAN
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