UPLC-MS/MS同时测定烟草中5种新烟碱杀虫剂残留  

Determination of Five Neonicotinoid Insecticide Residues in Tobacco by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：熊巍 张海燕 靳冬梅 韶济民 陶晓秋 庞夙 XIONG Wei;ZHANG Hai-yan;JIN Dong-mei;SHAO Ji-min;TAO Xiao-qiu;PANG Su(Sichuan Tobacco Quality Supervision and Testing Station,Chengdu 610041,PRC)

机构地区：[1]四川省烟草质量监督检测站,四川成都640001

出　　处：《湖南农业科学》2021年第2期91-95,共5页Hunan Agricultural Sciences

基　　金：四川省烟草专卖局(公司)科技计划项目(201301003)。

摘　　要：为寻求快速、高效、节本检测新烟碱杀虫剂残留量的方法,建立了吡虫啉,啶虫脒,烯啶虫胺,噻虫啉,噻虫胺5种新烟碱杀虫剂残留量的超高效液相色谱-串联质谱(UPLC-MS/MS)联用检测方法。烟叶样品经改进的QuEChERS提取处理后,使用Atlantis UPLC HSS T3反相柱,流动相为甲醇-水(含0.1%甲酸),用多反应监测模式测定,氘代内标法定量。此方法检测5种农药残留的线性关系良好,相关系数R~2>0.99,检出限分别为1.12、0.76、1.56、1.94、1.70 μg/kg,3个不同添加水平的加标回收率为69.3%~115.9%,相对标准偏差小于12%。采用该方法测定了63个国内外烟叶样品,结果显示:样品中吡虫啉和啶虫脒的检出率分别为11.1%和6.3%,平均含量分别为0.146和0.120 μg/g,其他指标均未检出。In order to develop a rapid,efficient,economic method for the determination of neonicotinoid insesticides residuces,the ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)was chosen for the determination of imidacloprid,acetamiprid,nitenpyram,thiacloprid and clothianidin residuces in tobacco.Samples were processed by modified QuEChERS,and extracts were separated on Atlantis UPLC HSS T3 column using methanol-water(containing 0.1%formic acid)as mobile phase.The neonicotinoid insecticides were determined by a tandem mass spectrometer with deuterated internal standard under multiple reaction monitoring mode.The above method showed a good linear relationship for the assay of the five insecticide residues(R^(2)>0.99).LODs of the five insesticides was 1.12,0.76,1.56,1.94,1.70μg/kg,respectively.The spike recoveries of 3 dosages of insecticide addition levels ranged from 69.3%to 115.9%with RSD less than 12%.This method was applied to determining the five neonicotinoid insesticides in 63 domestic and imported tobacco samples.The result showed that the detection rate of imidacloprild and acetamiprid residuces was 11.1%and 6.3%,averagely reaching 0.146μg/g and 0.120μg/g,respectively,while no other neonicotinoid insesticide residues were detected.

关 键 词：液相色谱-串联质谱 烟草 新烟碱杀虫剂 农残检测 

分 类 号：S481.8[农业科学—农药学]