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| Rapid Detection of Trace Amounts of Nitroimidazoles and Their Metabolites in Honey Using Liquid Chromatography Coupled with Quadrupole/Linear Ion Trap Mass Spectrometry |
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| DOI：10.3969/j.issn.1004-4957.年份.月份 |
| KeyWord:nitroimidazole metabolites residues honey liquid chromatography quadruple/linear ion trap mass spectrometry |
| Author | Institution |
| 张鸿伟，简慧敏，林黎明，陈亮珍，梁成珠，袁涛，汤志旭，蔡雪，秦良勇 |
1.山东出入境检验检疫局检验检疫技术中心;2.山东省检验检疫科学技术研究院;3.青岛蔚蓝生物集团有限公司;4.山东出入境检验检疫局 |
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| Abstract: |
| 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. |
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