超高效液相色谱-串联质谱法同时测定玉米和植株中苯唑草酮和莠去津残留

Simultaneous determination of topramezone and atrazine residues in corn and plant by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  玉米  植株  苯唑草酮  莠去津  残留

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  corn  plant  topramezone  atrazine  residues

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时测定玉米和植株中苯唑草酮和莠去津残留的分析方法。方法 样品经乙腈/水提取, C18和乙二胺-N-丙基硅烷化硅胶(primary secondary amine, PSA)分散固相萃取净化, 多反应监测(multiple reaction monitoring, MRM)模式下采用UPLC-MS/MS测定, 基质匹配外标法定量。结果 在0.0005~0.0500 mg/L范围内2种农药线性关系良好(r>0.999), 添加浓度为0.01~0.10 mg/kg时, 苯唑草酮在玉米和植株中的回收率为73.4%~97.8%, 相对标准偏差为2.2%~6.9%; 添加浓度为0.005~0.100 mg/kg时, 莠去津在玉米和植株中的回收率为74.2%~105.5%, 相对标准偏差为2.8%~14.8%。结论 该方法分离净化效果好、操作简便, 准确度和精密度均可满足残留检测要求。

英文摘要:

      Objective To establish a method for the simultaneous determination of topramezone and atrazine residues in corn and plant by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The sample was extracted by acetonitrile/water, cleaned-up by dispersive solid phase extraction with C18 and primary secondary amine (PSA), analyzed by UPLC-MS/MS under multiple reaction monitoring mode (MRM), and quantified by external standard method. Results In the range of 0.0005?0.0500 mg/L, the linear relationships between topramezone and atrazine were good, with r>0.999. When the concentrations were 0.01?0.10 mg/kg, the recoveries of oxazolidone in maize and plants were 73.4%?97.8%, and the relative standard deviations were 2.2%?6.9%; when the concentrations were 0.005?0.100 mg/kg, the recoveries of atrazine in maize and plants were 74.2%?105.5%, and the relative standard deviations were 2.8%?14.8%. Conclusion The method has good separation and purification effect, simple operation, and the accuracy and precision can meet the requirements of residue detection.