A rapid determination method for amantadine and rimantadine in swine urine was established using ultra performance liquid chromatography-electrospray tandem mass spectrometry(UPLC-ESI-MS/MS) in multiple reaction monitoring(MRM) mode.The urine sample was extracted with acetonitrile by ultrasonic,and cleaned up with solid-phase extraction Oasis MCX column.The separation of compounds was carried on an Eclipse Plus C18(RRHD 1.8 μm,2.1 mm×100 mm) by gradient elution using methanol-0.1% formic acid as mobile phase.The electrospray was operated in the positive mode and the samples were monitored under the multiple reaction monitoring(MRM) mode.The chromatographic retention time and mass fragment ion abundance ratio were taken for qualitative confirmation,and the internal standard method was employed for quantification analysis.The limits of detection(LOD) for both compounds were 0.05 μg/L,and the limits of quantitation(LOQ) were 0.2 μg/L in swine urine.The correlation coefficients of the swine urine were greater than 0.999(r2>0.999) within 0.2-20.0 μg/L linear ranges.Recoveries of amantadine and rimantadine at spiked levels of 0.5-20.0 μg/L were in the range of 89.7%-102.8% with intra-day relative standard deviation(RSDs) of 2.8%-4.2%.
关键词
超高效液相色谱-电喷雾串联质谱法(UPLC-ESI-MS/MS)金刚烷胺金刚乙胺猪尿
Keywords
ultra performance liquid chromatography-electrospray tandem mass spectrometry(UPLC-ESI-MS/MS)amantadinerimantadineswine urine
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宁波市农业科学研究院
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