药学研究2023，Vol.42Issue(12)：1000-1004,5.DOI:10.13506/j.cnki.jpr.2023.12.009
UPLC-MS/MS法测定磷酸西格列汀中基因毒性杂质NTTP
Determination of genotoxic impurity NTTP in Sitagliptin Phosphate by UPLC-MS/MS
摘要
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.关键词
磷酸西格列汀/基因毒性杂质/Nitroso-STG-19/含量测定/超高效液相色谱-串联质谱Key words
Sitagliptin Phosphate/Genotoxic impurity/NTTP/Content determination/UPLC-MS/MS分类
药学引用本文复制引用
袁松,李婕,张娜,张龙浩,刘阳,张庆生..UPLC-MS/MS法测定磷酸西格列汀中基因毒性杂质NTTP[J].药学研究,2023,42(12):1000-1004,5.基金项目
中国食品药品检定研究院关键技术研究基金(No.GJJS-2022-4-2) （No.GJJS-2022-4-2）
