气相色谱-负化学源质谱法测定蔬菜中17种拟除虫菊酯类农药残留量  

Determination of 17 pyrethroid pesticide residues in vegetables by gas chromatography-mass spectrometry with negative chemical ionization

作　　者：沈伟健[1] 曹孝文 刘一军[1] 张睿[1] 范欣[1] 赵增运[1] 沈崇钰[1] 吴斌[1] 

机构地区：[1]江苏出入境检验检疫局食品实验室,江苏南京210001 [2]常州出入境检验检疫局,江苏常州213022

出　　处：《色谱》2012年第11期1172-1177,共6页Chinese Journal of Chromatography

基　　金：国家质量监督检验检疫总局科技计划项目(2011KJ39;2012KJ31);科技部科技支撑项目(2011BAK10B04)

摘　　要：建立了气相色谱-负化学源质谱检测蔬菜中17种拟除虫菊酯类农药残留量的方法。样品中的目标物经乙腈提取后,用乙二胺-N-丙基甲硅烷(PSA)和石墨化炭黑填料进行分散固相萃取净化,气相色谱-负化学源质谱选择离子监测模式测定,同位素内标法定量。在甜豌豆、绿花菜和大葱基质中均未见干扰所有农药测定的现象。17种拟除虫菊酯类农药的定量限均为0.02～5μg/kg。在10、20、30和100μg/kg等4个添加水平下,所有农药的回收率均为71.0%～139.0%,相对标准偏差≤12.8%。该方法可作为蔬菜中17种菊酯类农残检测的确证方法。A method was established for the determination of 17 pyrethroid pesticide residues in vegetables using QuEChERS（quick,easy,cheap,effective,rugged and safe） clean-up method and gas chromatography-mass spectrometry（GC-MS） with negative chemical ionization（NCI）.The pyrethroid pesticides in the sample were extracted with acetonitrile.After QuEChERS clean-up with a mixture of primary secondary amine and graphitized carbon black packings,the extract was analyzed by GC-NCI-MS in selected ion monitoring（SIM） mode.An isotope internal standard of cypermethrin was employed to the quantification.The limits of quantification ranged from 0.02 to 5 μg/kg.The recoveries of the pyrethroid pesticides spiked in three different matrixes（peas,broccoli and Chinese onion green） at four spiked levels of 10,20,30 and 100 μg/kg were from 71.0% to 139.0%,and the relative standard deviations were less than 12.8%.This method can be used as a conclusive evidence method of the 17 pyrethroid pesticide residues in vegetables.

关 键 词：气相色谱 负化学离子源质谱 拟除虫菊酯类农药 蔬菜 

分 类 号：O658[理学—分析化学]