液相色谱-离子阱-飞行时间串联质谱快速筛查蔬菜中188种农药残留  

Rapid Determination of 188 Pesticide Residues in Vegetable by Liquid Chromatography-Ion Trap-Time of Flight Tandem Mass Spectrometry

作　　者：孙碧霞[1] 郭德华[2] 丁卓平[1] 冀峰 董吉川[2] 姚劲挺 

机构地区：[1]上海海洋大学食品学院,上海201306 [2]上海出入境检验检疫局,上海200135 [3]岛津国际贸易(上海)有限公司,上海200052

出　　处：《分析测试学报》2010年第10期1017-1024,共8页Journal of Instrumental Analysis

基　　金：上海应对技术性贸易措施专项资助项目(07TBT004);上海市教育委员会学科建设资助项目(J50704)

摘　　要：建立了蔬菜中188种农药多残留的液相色谱-离子阱-飞行时间串联质谱(LC-MS-IT-TOF)检测方法。样品以乙酸-乙腈(1∶99)提取,旋转蒸发近干后经活性炭和N-丙基乙二胺(PSA)复合固相萃取柱(CarbonGCB/PSASPE)净化,乙腈-甲苯(3∶1)洗脱,氮吹至干,甲醇定容后上机测定。除啶虫脒、联苯三唑醇、速灭磷的线性范围为10～250μg/L外,其余农药的线性范围均为5～250μg/L,相关系数均大于0.987,检出限为0.02～5.50μg/kg。在西兰花空白基质中进行5、10μg/kg两水平的加标回收实验,平均回收率分别为18%～105%、26%～130%,相对标准偏差分别为5.8%～30.1%、2.8%～22.8%。A multiresidue analytical method was developed for the determination of 188 pesticides in vegetable using liquid chromatography-ion trap-time of flight tandem mass spectrometry（LC-MS-IT-TOF）.The pesticide residues were extracted from samples by acetic acid-acetonitrile（1∶99,by volume）.The extract was cleaned up on a solid phase extraction column with complex carbon and N-propyl ethylenediamine（Carbon GCB/PSA SPE）,eluted with acetonitrile-toluene（3∶1,by volume）,evaporated with a stream of nitrogen near to dryness and redissoved by methanol.The separation of pesticides was performed on a Shimadzu Shim-pack XR-ODS Ⅱ（2.0 mm i.d.×75 mm,2.2 μm）by gradient elution with a flow rate of 0.4 mL/min at 40 ℃.The detections for pesticides were carried out under positive and negative electrospray ionization modes at the same time.The linear ranges for pesticides were 5-250 μg/L except for acetamiprid,bitertanol and mevinphos of 10-250 μg/L.The correlation coefficients were larger than 0.987 and the limits of detection ranged from 0.02 μg/kg to 5.50 μg/kg.The method was validated at two fortification levels of 5,10 μg/kg in broccoli,and the mean recoveries were in the range of 18%-105% and 26%-130%,respectively,with relative standard deviations（RSDs）of 5.8%-30.1%and 2.8%-22.8%,respectively.

关 键 词：液相色谱-离子阱-飞行时间串联质谱 多农药残留 蔬菜 

分 类 号：O657.63[理学—分析化学] F767.2[理学—化学]