OBJECTIVE To establish a high performance liquid chromatography-triple quadrupole/composite linear ion trap mass spectrometry method of two genotoxic impurities, 2-cyano-4’-bromomethyl biphenyl and 2-cyano-4’,4’-bisbromomethyl biphenyl, in the antihypertensive drug irbesartan.
METHODS After solvent dissolution, the samples were separated by Agilent Eclipse XDB-C18 column(2.1 mm×100 mm, 3.5 μm), eluted in gradient, and the eluate was detected by multiple reaction monitoring trigger enhancer ion scanning mode, qualitatively by second-level mass spectrometry and quantified by external standard.
RESULTS The detection and quantification limits of the two genotoxic impurities were 0.5 and 1.0 mg·kg−1, respectively, with good linear relationship between 1−20 μg·L−1(R2>0.999), at 1, 5 and 10 μg·L−1, the average recovery was between 90% and 110%, and the RSD was <5%.
CONCLUSION The established method is easy to operate, accurate in qualitative and quantitative analysis, and can meet the analysis needs of the two genotoxic impurities in irbesartan.
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