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Method for determining rivaroxaban and impurities thereof through adopting liquid chromatography

A technology of rivaroxaban and liquid chromatography, which is applied in the field of determination of impurities in rivaroxaban and its preparations by liquid chromatography, can solve problems such as the inability to realize effective quality control of rivaroxaban and its preparations, and achieve guaranteed The effect of quality control, improved resolution, and peak shape symmetry

Active Publication Date: 2016-07-06
CHONGQING PHARMA RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It solves the problem that the existing technology cannot realize effective quality control of rivaroxaban and its preparations, and the method can simply, quickly and accurately separate and detect related substances in rivaroxaban and its preparations, that is, impurities

Method used

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  • Method for determining rivaroxaban and impurities thereof through adopting liquid chromatography
  • Method for determining rivaroxaban and impurities thereof through adopting liquid chromatography
  • Method for determining rivaroxaban and impurities thereof through adopting liquid chromatography

Examples

Experimental program
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Effect test

Embodiment 1

[0060] Instruments and Conditions

[0061] Agilent1260 liquid chromatograph and chemical workstation; automatic sample injection; Kromasil100-5C18 column (5mm, 250×4.6mm) as separation column; UV detector wavelength: 250nm; mobile phase: 0.05% trifluoroacetic acid and 0.01 mol / L sodium dihydrogen phosphate mixed solution (adjust pH value to 4.50 with sodium hydroxide solution) as mobile phase A, acetonitrile as mobile phase B, gradient elution; 0 minutes, mobile phase A is 93% (V / V ), the mobile phase B is 7% (V / V); from 0 minutes to 9 minutes, the mobile phase A linearly decreases to 70% (V / V), and the mobile phase B linearly increases to 30% (V / V); 9 minutes From 28 minutes to 28 minutes, the mobile phase A linearly decreased to 60% (V / V), and the mobile phase B linearly increased to 40% (V / V); from 28 minutes to 50 minutes, the mobile phase A linearly decreased to 30% (V / V ), the mobile phase B increased linearly to 70% (V / V); 50.1 minutes, the mobile phase A was 93% (V / V)...

Embodiment 2

[0068] Determination of impurities in raw materials of rivaroxaban.

[0069] Take about 12.5mg of rivaroxaban, weigh it accurately, put it in a 25ml measuring bottle, add diluent (methanol: acetonitrile: water = 2:1:1V / V) and sonicate to dissolve and dilute to the mark, shake well, and use as Need testing solution; Precision measures need testing solution appropriate amount in addition, adds diluent and makes concentration and is the solution of need testing solution concentration 1.0%, as contrast solution; Carry out liquid chromatography analysis according to the chromatographic condition of embodiment 1, for If there are impurity peaks (except solvent peaks) in the chromatogram of the test solution, the peak area of ​​the known impurities multiplied by the correction factor shall not be greater than 1 / 2 (0.5%) of the main peak area of ​​the control solution, and the peak area of ​​a single impurity shall not be greater than that of the control The main peak area of ​​the so...

Embodiment 3

[0071] Determination of impurities in rivaroxaban tablets by liquid chromatography.

[0072] Take an appropriate amount of this product (approximately equivalent to rivaroxaban 12.5mg), put it in a 25ml measuring bottle, add a diluent (ethyl methanol: acetonitrile: water = 2:1:1V / V) and sonicate to dissolve and dilute to the mark. Shake well, as the test solution; in addition, accurately measure the appropriate amount of the test solution, add a diluent to make a solution with a concentration of 1.0% of the test solution, and use it as a control solution; Need testing solution identical method prepares blank adjuvant need testing solution; Carry out liquid chromatography analysis according to the chromatographic condition of embodiment 1, if impurity peak (except solvent peak and blank adjuvant peak) is arranged in the chromatogram of need testing solution, The peak area of ​​the known impurities multiplied by the correction factor shall not be greater than 1 / 2 (0.5%) of the m...

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Abstract

The invention discloses a method for determining rivaroxaban and impurities thereof through adopting liquid chromatography. The method is characterized in that rivaroxaban and impurities of a preparation thereof are determined by adopting a chromatographic column adopting octadecylsilane chemically bonded silica as a packing, a mixed buffer solution as a mobile phase A and acetonitrile as a mobile phase B through liquid chromatography, and gradient elution with the mobile phases is carried out. The method has the advantages of effective separation and determination of rivaroxaban and known and unknown impurities, strong specificity, high accuracy, simple operation, and effective control of the quality of rivaroxaban and the preparation thereof.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, in particular to a method for measuring impurities in rivaroxaban and its preparations by liquid chromatography. Background technique [0002] Rivaroxaban is an oral anticoagulant that directly inhibits factor Xa with high selectivity, and its molecular formula is C 19 h 18 ClN 3 o 5 S, whose structural formula is shown in the following formula (a) compound. [0003] [0004] The chemical name of rivaroxaban is: 5-?Chloro-?N-?({(5S)?-?2-?Oxo-?3-?[4-?(3-?Oxo-?4- ?Morpholinyl)?-?Phenyl]?-?1,?3-?Oxazolidine-?5-?yl}?-?Methyl)?-?2-?thiophene-carboxamide. In the process of synthesizing rivaroxaban, some intermediates of known structures and unknown impurities remain due to incomplete removal, which affects the purity and quality of rivaroxaban. These intermediates of known structures and impurities of unknown structures and The degradation products of varoxaban are collectively referred t...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/88
Inventor 冷飞覃柳洁王涛张道林石瑞娜邹春兰
Owner CHONGQING PHARMA RES INST
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