Simultaneous determination of two toxic impurities in the intermediate of dabigatran etexilate by UHPLC-MS with positive/negative ionization switching / 中国药学杂志
Chinese Pharmaceutical Journal
; (24): 930-934, 2016.
Article
en Zh
| WPRIM
| ID: wpr-859098
Biblioteca responsable:
WPRO
ABSTRACT
OBJECTIVE:
To determine two toxic impurities, namely bromoacetic acid and 4-aminobenzonitrile, in the intermediate of dabigatran etexilate by UHPLC-MS.METHODS:
The separation was performed on a Shimadzu Shim-Pack GIS C18 column (2.1 mm×50 mm, 2 μm) with mobile phase consisting of 0.1% formic acid aqueous solution (A) and 0.1% formic acid methanol (B) by gradient elution at a flow rate of 0.4 mL·min-1. The detection was achieved by triple quadrupole mass spectrometry with rapid polarity switching using MRM mode.RESULTS:
The calibration curves were linear in the ranges of 0.2-40 and 0.4-40 ng·mL-1 for bromoacetic acid and 4-aminobenzonitrile, respectively. The values of LOQ of bromoacetic acid and 4-aminobenzonitrile were 0.1 and 0.4 ng·mL-1, respectively. The recoveries of bromoacetic acid and 4-aminobenzonitrile were 100.9% and 99.6%, respectively.CONCLUSION:
The method is accurate, rapid, sensitive, and reliable to determine the two toxic impurities bromoacetic acid and 4-aminobenzonitrile in the intermediate of dabigatran etexilate for quality control.
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Base de datos:
WPRIM
Idioma:
Zh
Revista:
Chinese Pharmaceutical Journal
Año:
2016
Tipo del documento:
Article