分散固相萃取-超高效液相色谱-串联质谱联用快速检测玉米及土壤中莠去津残留

采用分散固相萃取（QuEChERS）为样品前处理方法,建立了超高效液相色谱-串联四极杆质谱快速检测玉米及土壤中莠去津残留分析方法。玉米及土壤样品经乙腈提取、乙二胺-N-丙基硅烷（PSA）分散固相（DSPE）净化后,应用超高效液相色谱/电喷雾串联四极杆质谱仪多离子反应监测（MRM）定量检测,分别以碎片离子m/z216〉146和m/z216〉174定性,以m/z216〉96进行外标法定量。结果表明,在0.005～0.5mg·kg^-1添加水平范围内莠去津的平均添加回收率在77.01%～112.62%之间,相对标准偏差在2.23%～8.43%之间,对莠去津的检出限（LOD）为0.39～0.91μg·kg^-1,定量检出限（LOQ）为1.33～3.02μg·kg^-1。该方法灵敏度高,操作简单,定量准确,测定浓度范围宽,可用于莠去津的残留分析。

Simplified Method for Determination of Atrazine Residues in Corn and Soil Using QuEChERS and UPLC-MS/MS

A rapid method for the determination of atrazine residues in corn and soil was established based on matrix solid-phase dispersion and ultraperformance liquid chromatography-mass spectrometry（UPLC-MS/MS）.The sample was extracted by acetonitrile and then purified by praimary secondary amine（PSA）.The atrazine residues was analyzed by UPLC-MS/MS under multiple reaction monitoring mode.The qualitative results were obtained based on retention time, the precursor ion and two daughter ions, and the quantitation results were on the intension of the characteristic 216146 ion 、m/z 216174 ion and m/z 21696 ion. Average recoveries of atrazine in soil and corn samples were found in the range of 77.01%～112.62% at three spiking levels from 0.005 mg·kg^-1 to 0.5 mg·kg^-1 with relative standard deviations of 2.23%～8.43%. Limits of detections of atrazine were 0.39～0.91 μg·kg^-1,while limits of quantifications were 1.33～3.02 μg·kg^-1, respectively.The method is simple and suitable for the routine and confirmation analysis.