Determination of N-nitrosodimethylamine and N-nitrosodiethylamine in agatroban by GC-MS/MS
Objective To simultaneously determine of N-nitrosodimethylamine(NDMA)and N-nitrosodiethylamine(NDEA)in agatroban by GC-MS/MS.Methods The sample was separated by Agilent DB-WAX UI chromatographic column(30 m×0.25 mm × 0.25 μm),while electron bombardment ionization source(EI)and the multiple reactive ion monitoring were selected for the dectection.A standard curve was established for the determination of both impurities in agatroban.Results NDMA and NDEA had good linearity at 19.20～128.00 ng·mL-1 and 5.36～35.73 ng·mL-1,respectively.The limit of quantification for NDMA and NDEA was 19.20 ng·mL-1 and 5.36 ng·mL-1.The limit of detection were 6.40 ng·mL-1 and 1.79 ng·mL-1,respectively.And the average recoveries of low,medium,and high concentration of NDMA and NDEA were 110.2％,107.8％,and 107.2％(RSD=3.2％,n=3),and 114.7％,107.3％,and 107.6％(RSD=5.6％,n=3),respectively.Conclusion This method is simple to operate,and can effectively detect the content of NDMA and NDEA in agatroban.
agatrobanGC-MS/MSN-nitrosodimethylamineN-nitrosodiethylaminemultiple reactive ion monitoring
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