咪鲜胺及2,4,6-三氯苯酚在牛奶中的残留检测方法

摘要

建立了牛奶中咪鲜胺及2,4,6-三氯苯酚残留的气相色谱质谱(GC-MS)检测方法.牛奶样品经乙腈-丙酮(7:3)提取,凝胶渗透色谱(GPC)净化,GC-MS检测,内标法定量.结果表明,在牛奶中咪鲜胺和2,4,6-三氯苯酚的定量限分别为0.05,0.025 mg,/kg;最小检出量分别为0.2,0.5 ng;咪鲜胺在牛奶中的平均回收率为82.6％～109.1％,相对标准偏差(RSDs)为1.7％ ～ 4.0％;2,4,6-三氯苯酚在牛奶中的平均回收率为85.3％～99.3％,相对标准偏差(RSDs)为2.6％～5.8％.该方法提取效果好,具有良好的回收率和重复性.%A gas chromatography and mass spectrometry (GC-MS) method was established for the determination of prochloraz and 2,4,6-trichlorophenol residues in milk.The milk samples were extracted with acetonitrile-acetone (7:3)solvent and purified by using GPC.The final extract was injected into GC-MS and quantified by internal standard method.The result showed that the limits of quantification (LOQs) were 0.05,0.025 mg/kg for prochloraz and 2,4,6-trichlorophenol,limit of detection of prochloraz and 2,4,6-trichlorophenol were 0.2,0.5 ng.The recoveries of prochloraz and 2,4,6-trichlorophenol spiked in milk were 82.6％-109.1％ and 85.3％-99.3％ with the relative standard deviations (RSDs) 1.7％-4.0％ and 2.6％-5.8％.The results show that the proposed method is sensitive and accurate for the determination of prochloraz and 2,4,6-trichlorophenol in milk.