Rapid Detection of Trace Amounts of Nitroimidazoles and Their Metabolites in Honey Using Liquid Chromatography Coupled with Quadrupole/Linear Ion Trap Mass Spectrometry
Rapid Detection of Trace Amounts of Nitroimidazoles and Their Metabolites in Honey Using Liquid Chromatography Coupled with Quadrupole/Linear Ion Trap Mass Spectrometry[J]. 2012,31(7):763-770.
Rapid Detection of Trace Amounts of Nitroimidazoles and Their Metabolites in Honey Using Liquid Chromatography Coupled with Quadrupole/Linear Ion Trap Mass Spectrometry[J]. 2012,31(7):763-770.DOI:
A procedure for the fast trace analysis of nitroimidazoles(including metronidazole,ronidazole,dimetridazole and ipronidazole) and their hydroxyl-metabolites(2-hydroxymethyl-1-methyl-5-nitroimidazole,hydroxymetronidazole,hydroxyipronidazole) was developed by liquid chromatography coupled with quadrupole/linear ion trap mass spectrometry.Honey samples were extracted with phosphate buffer(0.5 mol/L,pH 8.8)followed by liquid-liquid partition with ethyl acetate,and cleaned up by high speed freezing centrifugation.The separation of analytes was made on a C18 column using a mobile phase of 0.1% formic acid-methanol by gradient elution.A scheduled multiple reaction monitoring(sMRM) in positive mode as survey scan and an enhanced product ion(EPI) scan as dependent scan in an information-dependent acquisition(IDA) experiment was employed in mass spectrometry acquisition.Stable isotope-labeled analogues were used as the internal standards for quantitation.Confirmative analysis was performed through EPI spectra matching based on on-line lab-built library. Seven analytes showed good linearities in the range of 0.125-50.0 μg/L,with lower limits of detection(LLD) of 0.1 μg/kg for all analytes.At three fortification levels(1LLD,2LLD and 4LLD),the spiked recoveries ranged from 94% to 108% with RSDs no more than 11.4% under within-laboratory reproducibility conditions.The method was simple,rapid,sensitive and accurate,and could meet the requirements for routine analysis and residue surveillance control.
关键词
硝基咪唑代谢物残留蜂蜜液相色谱四极杆/离子阱质谱
Keywords
nitroimidazolemetabolitesresidueshoneyliquid chromatographyquadruple/linear ion trap mass spectrometry