高效液相色谱-串联质谱快速测定饲料中硝基咪唑类药物及其代谢物残留

发布时间：2018-12-11 19:29

【摘要】：建立了高效液相色谱-串联质谱快速测定饲料中甲硝唑(MNZ)、甲硝唑代谢物(MNZOH)、二甲硝咪唑(DMZ)、二甲硝咪唑代谢物(HMMNI)、洛硝哒唑(RNZ)、异丙硝唑(IPZ)、异丙硝唑代谢物(IPZOH)残留的分析方法。样品经0.1 mol/L pH 8.0磷酸盐缓冲液和乙酸乙酯-丙酮(70∶30)提取,提取液经分散型固相萃取填料N-丙基乙二胺(PSA)净化后,再经正己烷脱脂,液-液分配净化,采用电喷雾电离源(ESI)正离子多反应监测(MRM)模式检测,氘代同位素内标法定量。该方法省去耗时的固相萃取过程,快速、简单、高效,7种目标分析物在2.0~100.0μg/L范围内线性关系良好,相关系数大于0.99,在5.0~25.0μg/kg范围内,3个加标水平的回收率为72.4%~95.6%,相对标准偏差(RSD)均小于12.5%;检出限为2.5μg/kg,定量下限为5.0μg/kg。
[Abstract]:A high performance liquid chromatography-tandem mass spectrometry (HPLC / MS) method for the rapid determination of metronidazole (MNZ),) metabolites (MNZOH), dimethylimidazole (DMZ),) and dimethylimidazole metabolites (HMMNI), Lodidazole (RNZ), isopropanidazole (IPZ),) in feed was established. Determination of (IPZOH) residues of isopropanidazole metabolites. The samples were extracted by 0.1 mol/L pH 8.0 phosphate buffer solution and ethyl acetate acetone (70:30). The extracts were purified by N-propylethylenediamine (PSA), and then degreased by n-hexane. After liquid-liquid partitioning purification, the (MRM) mode was monitored by electrospray ionization source (ESI) positive ion multireaction, and the deuterium isotope internal standard was used to determine the quantity. The method is fast, simple and efficient. The linear relationship of 7 target analytes is good in the range of 2.0 ~ 100.0 渭 g / L, the correlation coefficient is greater than 0.99, and the correlation coefficient is in the range of 5.0 ~ 25.0 渭 g/kg. The recoveries of the three standard addition levels were 72.4 and 95.6.The relative standard deviation (RSD) was lower than 12.5; The detection limit was 2.5 渭 g / kg and the limit of quantification was 5.0 渭 g / kg.
【作者单位】：淮安出入境检验检疫局国家饲料安全检测重点实验室(淮安);江苏出入境检验检疫局动植物与食品检测中心;
【基金】：质检总局科技计划项目(2015IK131)
【分类号】：S816.17;O657.63

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