UPLC―MS―MS法快速测定大白菜和土壤中氰氟虫腙残留.docVIP

UPLC―MS―MS法快速测定大白菜和土壤中氰氟虫腙残留 　　摘要：建立大白菜和土壤中氰氟虫腙残留的超高效液相色谱-三重四极杆串联质谱（UPLC-MS-MS）快速检测的方法。样品用酸化乙腈提取、QuEChERS法净化，超高效液相色谱-串联质谱电喷雾正离子模式检测。结果表明，氰氟虫腙在5～500 μg/L范围内浓度和响应峰面积线性关系良好，相关系数为0.999。在0.005、0.01、0.05、0.2和1.0 mg/kg添加浓度下，平均回收率87.2%～113.4%，相对标准偏差（RSD）为0.6%～9.3%（n=5），氰氟虫腙在大白菜和土壤中的定量限（LQD）均为0.005 mg/kg。该方法适用于大白菜和土壤中氰氟虫腙的检测。 　　关键词：超高效液相色谱串联质谱（UPLC-MS-MS）；QuEChERS法；大白菜；土壤；氰氟虫腙 　　中图分类号：O657.63；O657.7+2；S481+.8 文献标识码：A 文章编号：0439-8114（2016）23-6231-04 　　DOI：10.14088/j.cnki.issn0439-8114.2016.23.058 　　Abstract：A method for the rapid determination of metaflumizone residues in Chinese cabbage and soil was developed by ultra high performance liquid chromatography-tandem triple quadruple mass spectrometry（UPLC-MS-MS）. Samples were extracted with acidified acetonitrile， purified by QuEChERS method and determined with UPLC-MS-MS positive electrospray ionization mode. The results showed that the metaflumizone had good linear relationship within the ranges of 5～500 μg/L between concentration and response peaks， and the correlation coefficient was 0.999. The average recoveries were in the range of 87.2%～113.4% when the additive concentration were 0.005， 0.01， 0.05， 0.2 and 1.0 mg/kg， the relative standard deviations were between 0.6% and 9.3%（n=5）. The limits of quantification were both 0.005 mg/kg in Chinese cabbage and soil. The method can be suitable for the determination of metaflumizone in Chinese cabbage and soil. 　　Key words：ultra high performance liquid chromatography-tandem mass spectrometry（UPLC-MS-MS）；QuEChERS method；Chinese cabbage；soil；metaflumizone 　　氰氟虫腙（Metaflumizone）化学名（E+Z）-2-[2-（4-氰基苯）-1-（3-三氟甲基苯）亚乙基]-N-（4-三氟甲氧基苯）联氨羰草酰胺，是20世纪90年代初日本Nohyaku公司发现的一种新型的缩氨基脲类杀虫剂，后来与德国巴斯夫公司联合开发出商品制剂艾法迪。它是一种钠离子通道阻抑杀虫剂[1]，本身具有杀虫活性，通过害虫取食进入体内，不需生物激活，以胃毒作用杀死害虫[2]，对咀嚼方式进食的鳞翅目幼虫以及鞘翅目幼虫和成虫具有良好的防治效果，对常见害虫，如甜菜夜蛾、小菜蛾、稻纵卷叶螟、菜青虫、斜纹夜蛾、棉铃虫以及马铃薯叶甲、黄条跳甲等，均有较好的效果[3-5]。 　　氰氟虫腙由于独特的化学结构和新颖的作用方式，尚未发现与其他种类的农药，如有机磷类、氨基甲酸酯类、拟除虫菊酯类等，存在交互抗性，同?r由于对有益生物影响小和对环境友好，被认为是低风险化合物，应用越来越广泛。国际上部分国家和组织，如国际食品法典委员会（CAC）、欧盟、