Determination of 4-Dimethylaminopyridine and Its N-Oxide in Tofogliflozin by LC-MS
A LC-MS method was established to determine the 4-dimethylaminopyridine(2)and 4-dimethyl-aminopyridine N-oxide(3)in tofogliflozin(1).The ACQUITY UPLC BEH C18 column(4.6 mm×150 mm,5 pm)was used,with the electrospray ionization and multiple response monitoring mode.The analysis was carried out in the gradient elution mode with methanol as mobile phase A,and 0.1％formic acid aqueous solution as mobile phase B.The results showed that it was linear for 2 and 3 in the ranges of 15.40-616.00 ng/mL and 15.58-623.20 ng/mL,respectively.The limits of detection for 2 and 3 were 3.08 and 3.12 ng/mL,respectively.The average recoveries were 104.33％and 101.54％,with RSDs of 3.32％and 3.10％,respectively.The established method is sensitive,selective and accurate,which can be used for the determination of 2 and 3 in 1.
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