Determination of five genotoxic impurities in clopidogrel besilate by UPLC-MS/MS
A method for the determination of five genotoxic impurities of benzenesulfonates in clopidogrel besilate was developed using ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)and comprehensive validation of the method was carried out.The results showed that the limits of quantification(LOQ)and limits of detection(LOD)of the method were low,with the LODs and LODs for p-nitrobenzenesulfonyl chloride(PNBSC)and p-nitrobenzenesulfonic acid(PNBA)being 0.045 ng/mL and 0.150 ng/mL,respectively,and those for p-nitrobenzenesulfonic acid(PNBAS)methyl ester(MES),p-nitrobenzenesulfonic acid(PNBSE)ethyl ester(EES)and p-nitrobenzenesulfonic acid(PNBS)isopropyl ester(IPE)being 0.113 ng/mL and 0.375 ng/mL,respectively.The five genotoxic impurities showed good linearity in their linear ranges with the correlation coefficients between 0.998 7 and 0.999 8,the RSD of the reproducibility ranged from 0.69％to 1.85％,and the recoveries of the spiked standards ranged from 82.98％to 119.92％.The method linearity,precision,accuracy,and durability met the requirements for quantitative analysis.Therefore,it is suitable for the determination of five genotoxic impurities in clopidogrel besilate.
ultra performance liquid chromatography-triple quadrupole mass spectrometry(UPLC-MS/MS)clopidogrel besilategenotoxic impurities
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