分析测试学报2012，Vol.31Issue(7)：763-770,8.DOI:10.3969/j.issn.1004-4957.2012.07.002
液相色谱-四极杆/离子阱质谱快速测定蜂蜜中痕量硝基咪唑类药物及其代谢物残留
Rapid Detection of Trace Amounts of Nitroimidazoles and Their Metabolites in Honey Using Liquid Chromatography Coupled with Quadrupole/Linear Ion Trap Mass Spectrometry
摘要
Abstract
A procedure for the fast trace analysis of nitroimidazoles (including metronidazole, ronidazole, dimetridazole and ipronidazole) and their hydroxyl-metabolites (2-hydroxymethyl-l-methyl-5-nitroimid-azole, 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 per-formed 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 ana-lytes. At three fortification levels(1LLI), 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Key words
nitroimidazole/ metabolites/ residues/ honey/ liquid chromatography/ quadruple/linear ion trap mass spectrometry分类
化学化工引用本文复制引用
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..液相色谱-四极杆/离子阱质谱快速测定蜂蜜中痕量硝基咪唑类药物及其代谢物残留[J].分析测试学报,2012,31(7):763-770,8.基金项目
国家质检总局科技项目(20071K144) （20071K144）
山东省科技发展计划项目(2008GG100009020) （2008GG100009020）
山东出入境检验检疫局科研攻关项目(SK200820) （SK200820）
