摘要
建立了高效液相色谱-电喷雾串联质谱（HPLC-ESI MS/MS）快速测定水产品中硝基咪唑类兽药甲硝哒唑（MNZ）、洛硝哒唑（RNZ）、迪美硝唑（DMZ）及其代谢物羟基甲硝唑（MNZOH）、羟基二甲硝咪唑（HMMNI）残留量的分析方法。样品在弱碱性条件下（磷酸二氢钠缓冲液,p H 8.0）经甲醇-丙酮（3∶1）混合液提取,乙酸乙酯萃取和乙腈正己烷分配脱脂净化;以0.1%甲酸水溶液和0.1%甲酸乙腈溶液为流动相,梯度洗脱,Agilent ZORBAX SB C18RRHD（100 mm×2.1 mm,1.8μm）色谱柱分离;多反应监测正离子模式扫描,同位素稀释内标法定量。结果表明,5种目标分析物在0.25-50μg/L范围内线性关系良好,相关系数为0.998 6-0.999 7;定量下限（S/N≥10）均可达到0.1μg/kg。各基质在0.1,0.5,10.0μg/kg加标水平的回收率为70.7%-105.1%,相对标准偏差为1.7%-8.1%。该方法操作快速、高效、定量重复性好,适用于水产品中硝基咪唑类药物残留的检测。
A liquid chromatography-tandem mass spectrometric（LC-ESI MS/MS） method was developed for the simultaneous determination of nitromidazoles and their metabolites residues,including metronidazole（MNZ）,ronidazole（RNZ）,dimetridazole（DMZ）,metronidazole-OH（MNZOH） and 2-hydroxymethyl-1-methyl-5-nitroimidazole（HMMNI） or dimetridazole-OH（DMZOH） in aquatic products.Samples were homogeneously extracted with methanol-acetone（3∶1） in 0.5 mol/L sodium dihydrogen phosphate（NaH2PO4） solution（pH 8.0）.The supernatant solution was concentrated by rotary evaporation followed by liquid-liquid partition with ethyl acetate.The fat was removed by acetonitrile-hexane distribution.The analytes were separated on a C18 column（Agilent ZORBAX SB C18 RRHD,100 mm×2.1 mm,1.8 μm） by gradient elution using a mobile phase of 0.1% formic acid solution and acetonitrile containing 0.1% formic acid,and detected by LC-ESI MS/MS under multiple reaction monitoring mode（MRM） via positive electrospray ionization（ESI＋）.Isotope dilution internal standard method was used for quantitation analysis.The results showed that the calibration curves of five kinds of compounds were linear in a certain concentration range（0.25-50 μg/L） with correlation coefficients of 0.998 6-0.999 7.The limits of quantitation（LOQs,S/N≥10） were 0.1 μg/kg.The average recoveries at three spiked levels of 0.1,0.5,10.0 μg/kg were between 70.7% and 105.1% with relative standard deviations（RSDs） of 1.7%-8.1%.The method showed advantages of rapidness,efficiency and high repeatability,and could meet the requirements for determination of nitromidazole residues in aquatic products.
出处
《分析测试学报》
CAS
CSCD
北大核心
2015年第1期28-34,共7页
Journal of Instrumental Analysis
基金
福建省科技厅青年创新项目(2012J05020)
关键词
液相色谱-串联质谱法
硝基咪唑
代谢物
水产品
残留
liquid chromatography - tandem mass spectrometry
nitromidazole
metabolite
aquatic product
residue
