气相色谱-负化学源质谱联用法测定菊酯类农药  

Determination of Pyrethroid Pesticide Residues by Gas Chromatography-Negative Chemical Ionization Mass Spectrometry and Its Application

作　　者：沈崇钰[1] 沈伟健[1] 蒋原[1] 徐锦忠[1] 赵增运[1] 陈惠兰[1] 吴斌[1] 

机构地区：[1]江苏出入境检验检疫局食品实验室,南京210001

出　　处：《分析化学》2006年第U09期36-40,共5页Chinese Journal of Analytical Chemistry

基　　金：江苏省科技攻关(农业)(No.BE2003345)资助项目

摘　　要：通过固相萃取-气相色谱-负化学离子源质谱技术建立了11种拟除虫菊酯类农药残留的检测方法，并应用于茶叶农残检测。样品经乙酸乙酯提取后，用串联的活性炭和中性氧化铝固相萃取柱选择性地富集茶叶中待测组分，再由气相色谱-负化学离子源质谱分时段选择离子监测技术进行测定。方法简单快速，一次进样就能得到11种菊酯残留结果；准确度和精密度高，在0．016μg／kg、0．032μg／kg和0．064μg／kg3个添加水平下的回收率在70％～110％之间，CV≤7．4％；选择性好，消除了色素和其它杂质干扰；灵敏度高，检出限低，除了氯菊酯为10μg／kg外，其它菊酯检出限都在μg/∥kg级，七氟菊酯则达到了0．02μg／kg。A solid phase extraction（SPE）-gas chromatography（GC）-negative chemical ionization mass spectrometry（NCI/MS） method was proposed for analyzing 11 kinds of pyrethroid pesticides in tea. Pesticide residues were extracted from tea samples with ethyl acetate. And extract was cleaned-up by active carbon SPE column connected to alumina neutral SPE column. Analytical screening was determined by the technique of gas chromatography-negative chemical ionization mass spectrometry-selected ion monitoring. The recoveries of all pyrethroid pesticides were in the range of 70% - 110% at three spiked level, 0.016, 0.032 and 0.064 μg/kg, and the relative standard deviations were below 7.4%. The limit of detections of all pesticides were from 0. 02 to 10 μg/kg. The method is reliable and stable.

关 键 词：气相色谱-负化学离子源质谱 选择离子监测 固相萃取 拟除虫菊酯 茶叶 

分 类 号：O657.63[理学—分析化学] TQ450.7[理学—化学]