Determination of genotoxic impurity NTTP in Sitagliptin Phosphate by UPLC-MS/MS
YUAN Song
LI Jie
ZHANG Na
ZHANG Longhao
LIU Yang
ZHANG Qingsheng
Abstract：Objective To establish an UPLC-MS/MS method for determination of genotoxic impurity Nitroso-STG-19(NTTP)in Sitagliptin Phosphate.Methods The separation of NTTP was performed on a Eclipse Plus C18 RRHD(3.0 mm×150 mm,1.8 μm)with the mobile phase consisting of 0.1%formic acid aqueous solution(mobile phase A)and 0.1%formic acid methanol solution(mobile phase B)under a gradient elution at a flow rate of 0.35 mL·min-1 and a column tem-perature of 30℃.Multiple reaction monitoring(MRM)was performed on a triple quadrupole mass spectrometer in positive mode.Results The calibration curves was in good linearity in the range of 0.54～53.93 ng·mL-1.The limit of detection was 0.02 ng·mL-1,and the limit of quantification was 0.08 ng·mL-1.The recoveries(n=3)of active pharmaceutical ingredients(API)and tablets at low,middle,and high spiked concentrations were 105.43%～107.21%(RSD≤3.2%)and 115.03%～120.20%(RSD≤3.6%)respectively.Using the developed method,we detected NTTP in 12 batches of API and 3 batches of preparation.The results showed that NTTP was detected in all batches.Conclusion The method was sensitive and accurate,which can be applied for the quantifications of NTTP in Sitagliptin Phosphate,providing reference for quality control of Sita-gliptin Phosphate.
Keywords：Sitagliptin PhosphateGenotoxic impurityNTTPContent determinationUPLC-MS/MS
Publication Date：2023-12-28
Online Publishing Date：2025-08-15(First online date of this platform, not the publication date of the document)
Pages：5( 1000-1004 )