Simultaneous Determination of Five Small Molecule Antivirals Including Nematovir in Pharmaceuticals by High Performance Liquid Chromatography-Tandem Mass Spectrometry
A HPLC-MS/MS method was established for the simultaneous detection of five small molecule antivirals,namely nirmatrelvir,ritonavir,molnupiravir,oseltamivir and daclatasvir.Samples were extracted by methanol with ultrasound extraction,and separated on a CNWShell C18 Core-Shell column(100×2.1 mm,2.6 μm)by gradient elution using 0.1％formic acid solution and methanol as the mobile phase.The electrospray ion source was operated in the positive ion mode and both multiple reaction monitoring and product ion scanning were used in this method.There were good linearities for five small molecule antivirals in their linear ranges.The limits of detection(LODs)were 0.15-0.5 μg/g and the limits of quantitation were 0.5-1.2 μg/g.Average recoveries of three spiked levels ranged from 90％to 97.4％(n=6)with the relative standard deviations(RSDs)less than 5％.The method was used to test 10 samples and 7 samples were found not to contain the active ingredient nirmatrelvir as labelled.Active ritonavir was found to be much lower than labelled,and illegally added chemicals such as oseltamivir or daclatasvir were detected.The method was proved to be sensitive,rapid and accurate for the qualitative and quantitative analysis of 5 small-molecule antivirals.
万方数据
维普
