[关键词]
[摘要]
建立了QuEChERS-液相色谱-串联质谱(LC-MS/MS)测定果蔬中新型杀虫剂氟吡呋喃酮残留量方法,通过分析样品提取净化液中基质干扰物,优化了分散吸附剂组合。采用1:2稀释样品液有效降低或消除基质效应,可直接采用溶剂标准溶液外标法进行定量分析,而无需采用基质匹配标准溶液或同位素内标以补偿基质效应。应用优化的方法,目标农药在苹果、橙、西红柿、菠菜、甜玉米、毛豆中3个添加水平(4、8、40 μg/kg)的回收率范围为80.90%~100.15%,相对标准偏差为3.56%~12.88%,方法的定量限(S/N>10)为4.00 μg/kg、基质效应绝对值均小于10%。本文方法灵敏、简便、准确,适用于果蔬中氟吡呋喃酮残留的快速测定,可为LC-MS/MS定量分析基质效应的消除提供参考。
[Key word]
[Abstract]
A fast method was developed for the determination of a novel insecticide (flupyradifurone) in fruits and vegetables using QuEChERS combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS). By analyzing the matrix interferents in the sample extraction purification solution, the combination of dispersed adsorbents was optimized. Using 1:2 diluted sample solution could effectively reduce or eliminate the matrix effects, and the external standard method of solvent standard solution could be directly used for quantitative analysis, without the need to use matrix-matched standard solution or isotope internal standard to compensate the matrix effects. Using the optimized method, the recoveries at fortification levels of 4, 8, and 40 μg/kg in apples, oranges, tomatoes, spinach, sweet corn and green soybeans ranged from 80.90% to 100.15% with relative standard deviations of 3.56% to 12.88%. The limits of quantification (S/N > 10) were 4 μg/kg, and the absolute matrix effects of all matrices was below 10%. The method has been shown to be sensitive, simple, accurate, and suitable for the rapid determination of flupyradifurone in fruits and vegetables and to be a methodological approach for the minimization of matrix effects in LC-MS/MS quantitative analysis.
[中图分类号]
[基金项目]
福建省自然科学基金项目(2016J01070);原国家质检总局项目(2017IK041)