Determination of N-nitrosamines Genotoxic Impurities in VaIsartan and Amlodipine Tablets(Ⅰ)by GC-MS/MS
A gas chromatography-tandem mass spectrometry(GC-MS/MS)method was established for the determination of two genotoxic impurities,N-nitrosodimethylaminen(NDMA)and N-nitrosodiethylaminen(NDEA),in valsartan and amlodipine tablets(I).The separation was carried out on an Agilent DB-WAXms(30 m×0.25 mm,0.25 μm)capillary column with programmed temperature increase,carrier gas flow rate of 3 mL/min and injection volume of 3 μL.The mass spectrometry analysis was performed using an electron bombardment(EI)ion source in multiple reaction monitoring(MRM)mode,and quantified by external standard method.The results showed that the separation between NDMA,NDEA and adjacent peaks was good,and the linearity was good in the ranges of 0.25 ng/mL～100 ng/mL for NDMA and 0.1 ng/mL～50 ng/mL for NDEA.The limits of quantification(LOQ)for NDMA and NDEA were 0.2 ng/mL and and 0.3 ng/mL respectively,and the limits of detection(LOD)were 0.07 ng/mL and The RSD of precision,reproducibility and stability tests were less than 8%,and the average recoveries were 91.2%～98.1%for NDMA and 89.9%～96.3%for NDEA.The method is sensitive,exclusive,with high recovery,wide linear range,easy and fast to operate,and can be used for the determination of NDMA and NDEA in valsartan and amlodipine tablets(Ⅰ).
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