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Method for determining apixaban cleaning residues by high performance liquid chromatography

A high-performance liquid chromatography and apixaban technology, which is applied in the field of high-performance liquid chromatography for the determination of apixaban cleaning residues, can solve the problems of irrelevant reports of trace residues, and achieve improved peak shape and effective detection of trace residues , Improve reliability, reduce the effect of detection limit

Active Publication Date: 2015-01-28
JIANGSU BAOZONG & BAODA PHARMACHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there is no pharmacopoeia and related literature in China to propose a detection method for this substance, and there is no relevant report on the detection of trace residues.

Method used

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  • Method for determining apixaban cleaning residues by high performance liquid chromatography
  • Method for determining apixaban cleaning residues by high performance liquid chromatography
  • Method for determining apixaban cleaning residues by high performance liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Determination of Apixaban Cleaning Residue Method by High Performance Liquid Chromatography:

[0033] Instruments and reagents: LC-2010A high performance liquid chromatography (quaternary pump, degassing unit, UV detector, column oven, automatic sampler, system monitor, LCsolution) (Shimadzu Corporation of Japan); (Manufacturer: Jiangsu Baozhong Baoda Pharmaceutical Co., Ltd., acetonitrile, methanol (Merck chromatographically pure), other reagents are analytically pure, and water is self-made fresh redistilled water.

[0034] Chromatographic condition selection: chromatographic column: Inertsil ODS-3V 5μm 250×4.6mm; mobile phase A: 30mmol / L ammonium acetate aqueous solution, mobile phase B: acetonitrile, isocratic elution; detection wavelength: 280nm; calculation method: external standard method ;Flow rate: 1.0 mLmin -1 ; Sensitivity: 1.0 AUFS; Injection volume: 10 μL; Column temperature: 40°C.

[0035] Specificity test: Methanol for rinsing of the sampling equipment,...

Embodiment 2

[0047] The precision test of the inventive method:

[0048] System precision: Take the control solution, inject 6 consecutive samples, and calculate the retention time and RSD of the peak area of ​​apixaban. The RSD of the actual measured retention time is 0.03%; the RSD of the peak area is 0.59%

[0049] Method precision: 6 control solutions were prepared repeatedly, and each solution was injected once. The RSD of peak area / weighted sample volume of apixaban was 0.68%.

[0050] Intermediate precision: The method precision test was repeated by another analyst on another day on another instrument, and the RSD of the peak area / weighted sample volume of apixaban was 6.87%.

[0051] It shows that the reproducibility is good and the method is reliable.

Embodiment 3

[0053] The limit of detection test of the inventive method:

[0054] By injecting a low concentration of apixaban reference substance solution, when the signal-to-noise ratio (S / N) is 3, this concentration is its detection limit, and the detection limit solution is injected for 3 injections, and the RSD of the peak area is calculated and reported. Finally, the concentration of 0.0125ug / ml when S / N was determined to be about 2.8 was the limit of detection. The area RSD was 4.6%.

[0055]

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Abstract

The invention relates to a method for determining apixaban cleaning residues by high performance liquid chromatography, and belongs to the field of chemical pharmaceutical detection. The invention aims at providing a method for determining the apixaban cleaning residues. The method is easy and quick to operate and accurate and reliable in determination results to evaluate a cleaning effect so as to ensure medicine quality and medication safety. The high performance liquid chromatography for determining the apixaban cleaning residues, which is disclosed by the invention, is easy and quick to operate, and accurate and reliable in the determination results, so that the cleaning effect of the equipment can be evaluated effectively. According to the high performance liquid chromatography, a 280 nm flow phase is selected, so that the detection limit is reduced effectively. A chromatographic column temperature selects 40 DEG C, so that the peak type can be improved effectively, and minimal residues can be effectively detected; methanol is selected to serve as a solvent, and is not absorbed in the wavelength, so that the interference on the detection caused by the solvent is avoided, and the reliability of the detection method is improved.

Description

technical field [0001] The invention relates to a high-performance liquid chromatography method for determining the cleaning residue of apixaban, belonging to chemical [0002] field of pharmaceutical testing. Background technique [0003] The raw material drug production process inevitably involves the problem of shared equipment. If the equipment is switched during the shared link, if the equipment is not cleaned completely, the residue of the material from the previous production will inevitably be brought into the next production. Due to the difference in drug toxicity, The size of the residue will directly affect the safety and quality of the drug, so it is very necessary to control the cleaning residue to a reasonable limit, and it is also required by the GMP regulation as the minimum pharmaceutical requirement. Generally, impurities are allowed to exist in the product within the allowable range of safety. Therefore, it is very necessary and urgent to use a certain in...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 丁海宏王琳张智红
Owner JIANGSU BAOZONG & BAODA PHARMACHEM
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