Determination of genotoxic impurity of suifonate ester in sildenafil citrate by LC-MS/MS
Obiective To establish an liquid chromatography mass spectromete (LC-MS/MS) method for the determination of genotoxic impurity ethyl 4-ethoxy-3-formylbenzenesulfonate in sildenafil citrate. Methods The separation was carried out on Agilent Poroshell 120 EC-C18 column (150 mm×2.1 mm,2.7 μm) at the column temperature of 25 ℃. The mobile phase was 0.1％ formic acid solution-methanol with gradient elution,the flow rate was 0.3 mL/min and the injection volume was 5 μL. The mass spectrometry was operated in electrospray ionization with multiplereactions monitoring mode .The quantitative ion pairs were m/z 259.3→203.1 and m/z 259.3→187.1. Results Ethyl 4-ethoxy-3-formylbenzenesulfonate had a good linear relationship within the concentration range of 4.92-196.99 ng/mL (r=0.9995). Its average recovery rate was 96.5％,and the RSD was 4.2％ (n=9). The detection limit was 0.098 ng/mL and the quantification limit was 0.246 ng/mL. Conclusion The method is simple,sensitive and reliable,which can be applied to determine genotoxic impurity ethyl 4-ethoxy-3-formylbenzenesulfonate in sildenafil citrate.
Sildenafil citrateGenotoxic impuritySuifonate esterEthyl 4-ethoxy-3-formylbenzenesulfonateHigh performance liquid chromatography mass spectromete
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