分散固相萃取-气相色谱串联质谱法测定大米中的毒死蜱、三环唑和戊唑醇残留  

Determination of Chlorpyrifos, Tricyclazole and Tebuconazole Residues in Rice by Gas Chromatography-tandem Mass Spectrometry Combined QuEChERS Method

作　　者：张娟 汪杰 姚成虎[1] ZHANG Juan;WANG Jie;YAO Cheng-hu(Ma＇an shah institute of Product Quality Supervision and Inspection,Laboratory of Agricultural Product Quality Inspection,Ma＇anshan 243000,Anhui,China)

机构地区：[1]马鞍山市产品质量监督检验所马鞍山市农产品质量安全监督检测中心,安徽马鞍山243000

出　　处：《农药》2018年第11期823-825,847,共4页Agrochemicals

摘　　要：[目的]建立同时测定大米中毒死蜱、三环唑和戊唑醇残留的气相色谱串联质谱(GC-MS/MS)方法。[方法]大米样品用乙腈提取,分散固相萃取净化,在多反应监测(MRM)模式下进行质谱检测,外标法定量。[结果]在0.05～1.0 mg/L质量浓度范围内线性关系良好,大米中毒死蜱、三环唑、戊唑醇的检出限分别为0.005、0.005、0.016mg/kg,定量限分别为0.018、0.016、0.054 mg/kg。在0.05～1.0 mg/kg添加水平下,大米中毒死蜱、三环唑和戊唑醇的平均回收率在82.4%～103.2%之间,相对标准偏差(RSD)均小于10%。[结论]该方法简单可靠、重现性好、灵敏度高,适合大批量样品的检测。[Aims] An analytical method for simultaneous determination of chlorpyrifos, tricyclazole and tebuconazole residues in rice by gas chromatography-tandem massspectrometry（GC-MS/MS） was developed. [Methods] The rice samples were extracted with acetonitrile, and then purified by the dispers solid-phase extraction. The target compounds were determinated under multiple reaction monitoring（MRM） mode and quantified by external standard method.[Results] Good linearity was obtained at 0.05-1.0 mg/L. The limits of detection for chlorpyrifos, tricyclazole and tebuconazole in rice were 0.005, 0.005 and 0.016 mg/kg, and the limits of quantitation were 0.018, 0.016 and 0.054 mg/kg,respectively. The average recoveries at the spiked levels of 0.05-1.0 mg/kg were in the range of 82.4 to 103.2%, and the relative standard deviations（RSDs） were less than 10%. [Conclusions] The method is simple and reliable, with good reproducibility and sensitivity, which is applicable for the detection of large numbers of samples.

关 键 词：气相色谱串联质谱 分散固相萃取 大米 毒死蜱 三环唑 戊唑醇 

分 类 号：TQ450.2[化学工程—农药化工]