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.
出处
《色谱》
CAS
CSCD
北大核心
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)
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
gas chromatography（GC）
negative chemical ionization mass spectrometry（NCI-MS）
pyrethroid pesticides
vegetables
