论文部分内容阅读
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。
A rapid method for the determination of metronidazole (MNZ), metronidazole metabolites (MNZOH), dimethyldiazepine (DMZ), methotrexate metabolites (HMMNI) and nitrofurantoin in feed was established by high performance liquid chromatography-tandem mass spectrometry (RNZ), isoquitazine (IPZ) and isozmerazine metabolites (IPZOH). The sample was extracted with 0.1 mol / L pH 8.0 phosphate buffer and ethyl acetate-acetone (70:30), and the extract was purified by dispersive solid-phase extraction packing N-propyl ethylenediamine (PSA) Alkane degreasing and liquid-liquid partitioning were used. The electrospray ionization source (ESI) positive ion multiple reaction monitoring (MRM) mode was used for the determination. The deuterated isotope internal standard method was used for quantification. The method eliminates the time-consuming solid-phase extraction process and is fast, simple and efficient. The linearity of the seven target analytes in the range of 2.0-100.0μg / L is good with a correlation coefficient greater than 0.99 and in the range of 5.0-25.0μg / kg The recoveries of three spiked levels were 72.4% -95.6% with relative standard deviations (RSDs) less than 12.5%. The detection limit was 2.5μg / kg and the limit of quantification was 5.0μg / kg.