Method for determining impurity content of apixaban by virtue of high performance liquid chromatography

A high-performance liquid chromatography and apixaban technology, which is applied in the field of high-performance liquid chromatography for determining the impurity content of apixaban, and achieves the effects of accurate and reliable determination results and simple operation.

Inactive Publication Date: 2018-05-04
JIANGSU BAOZONG & BAODA PHARMACHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Method for determining impurity content of apixaban by virtue of high performance liquid chromatography
  • Method for determining impurity content of apixaban by virtue of high performance liquid chromatography
  • Method for determining impurity content of apixaban by virtue of high performance liquid chromatography

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Embodiment 1

[0017] The method specificity test of the present invention:

[0018] Examine the specificity of the method by injecting the test solution containing all potential impurities as the specific solution. Determine the relative retention time and separation degree of each potential impurity under the determination conditions through the specificity test, to ensure that the impurities of concern can be detected, to ensure that the blank solution has no interference at the retention time of apixaban and impurities, and to ensure that the apixaban The peak purity of Banfeng is pure.

[0019] Result: In the blank solution, there is no interference peak at the retention time of the impurity and apixaban peaks; in the specific solution, all peaks should be separated from the known impurities and apixaban peaks, each known impurity and apixaban peak The separation degree of its adjacent peak is ≥1.5; in the test solution under degradation conditions, the separation degree between two re...

Embodiment 2

[0025] The system suitability test of the inventive method:

[0026] On every working day during the method validation, the system suitability test is carried out before the validation starts. Report system suitability results, with retention times for known impurities and apixaban. In the system suitability solution tested every day, the tailing factor of the apixaban peak should not be greater than 1.5; in the control solution, the theoretical plate number of the apixaban peak should not be lower than 40,000, and the signal-to-noise ratio should not be lower than 30.

[0027] .

Embodiment 3

[0029] The accuracy test of the inventive method:

[0030] The accuracy of the method is achieved by examining the accuracy of adding different concentrations of known impurities to the sample. Investigate the concentration of known impurities including quantification limit concentration (6 parts), 0.5μg / ml known impurities (0.05%), 1.0μg / ml known impurities (0.10%), 1.5μg / ml known impurities (0.15%) , each concentration was repeated 3 times, and the concentrations of unknown impurities were investigated, including the limit of quantification, 0.5 μg / ml apixaban (0.05%), 1.0 μg / ml apixaban (0.10%), 1.5 μg / ml apixaban Shaban (0.15%), each concentration was repeated 3 times. When the concentration is 0.10% and 0.15% of the normal detection concentration, the relative standard deviation (RSD) of the accuracy result is ≤15%, and the accuracy result should be 100±15%; when the concentration is 0.05% of the normal detection concentration, the relative standard deviation (RSD) of th...

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Abstract

The invention discloses a method for determining the impurity content of apixaban by virtue of a high performance liquid chromatography. The method is specifically characterized in that an Agilent 1200 series high performance liquid chromatograph is matched with a DAD detector and an automatic feeder, an Inertsil ODS-3V, 5-micron, 250*4.6mm chromatographic column is adopted for work for 32 minutesin a gradient manner, and the working conditions are as follows: the column temperature is 40 DEG C, the feeding amount is 10 microliters, the detection wavelength is 230nm, and the flow speed is 1.5ml/min. The analysis method is good in specificity, and an impurity BMS-591455 has good linearity in the range of 0.5microg/ml-1.5microg/ml. The method has the advantages of simplicity and rapidness in operation, reliable determination result and the like, the impurity content can be effectively controlled, and the quality of an apixaban drug can be controlled.

Description

[0001] The invention relates to a method for determining the impurity content of apixaban by high-performance liquid chromatography, which belongs to the field of chemical detection. Background technique [0002] Apixaban is a factor Xa inhibitor, suitable for the prevention and treatment of blood clots. In 2011, apixaban was the first to be approved in 27 EU countries, Iceland and Norway for the prevention of venous thrombosis in adult patients undergoing elective hip or knee replacement surgery; in January 2013, it was approved by the State Food and Drug Administration of China Import drug license, officially launched in China in April 2013. It is an anticoagulant drug with a new mechanism of action. The results of clinical trials confirmed that apixaban significantly reduced the primary endpoint - the incidence of all VTE / all-cause death composite endpoints, as well as major VTE endpoint events - proximal deep vein thrombosis (DVT), non-fatal pulmonary embolism (PE) And t...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 陈荣王琳倪林明
Owner JIANGSU BAOZONG & BAODA PHARMACHEM
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