程序升温汽化-气相色谱-三重四极杆串联质谱法(PTV-GC-MS/MS)同时测定小麦中的109种农药残留  

Simultaneous Determination of 109 Pesticide Residues in Wheat by PTV-GC-MS/MS

作　　者：袁河 赵振宇 吴建霞 王垄 聂叶 汪地强 王莉 高川川 楼小华 

机构地区：[1]贵州茅台酒股份有限公司技术中心,贵州仁怀564501 [2]贵州省烟草质量监督检测站,贵州贵阳550025

出　　处：《酿酒科技》2016年第6期120-128,共9页Liquor-Making Science & Technology

基　　金：国家科技支撑计划项目(2011BAC06B12);"863计划"项目(2013AA102108);贵州省重大科技专项合作项目(黔科合重大专项字(2013)6009号)

摘　　要：建立了一种同时测定小麦中109种农药残留（121个组分）的程序升温汽化-气相色谱-三重四极杆串联质谱（PTV-GC-MS/MS）检测方法。小麦样品经Qu ECh ERS技术快速提取与净化,PTV进样后在毛细管柱TR-pesticide II上分离,以保留时间窗口和特征SRM（选择性反应监测）离子对定性、峰面积定量。结果表明：（1）109种农药在小麦中的检出限（LOD）为0.6～10.6μg/kg,定量限（LOQ）为2.1～35.5μg/kg;（2）在1～950μg/L范围内,线性相关系数为0.9956～1.0000;（3）在小麦样品中添加浓度在7.3～620μg/kg之间时,平均回收率在66.6%～118.2%之间,RSD为1.0%～18.0%;（4）该方法对农药品种覆盖面广、前处理简单快速、节省溶剂,一次进样可分析109种农药,准确、灵敏。A method had been developed for simultaneous determination of 109 pesticides（121 components）in wheat by programmed temperature vaporizer gas chromatography with tandem mass spectrometry（PTV-GC-MS/MS）.The pesticide residues in wheat sample were extracted rapidly and purified with Qu ECh ERS technique, then separated on TR-pesticide II capillary chromatographic column after PTV sampling. Qualitative and quantitative analysis was conducted by retention time window and SRM（selective reaction monitoring） ion pairs with peak area respectively. The result showed that：（1）The limits of detection（LODs） of 109 pesticides were ranged from 0.6 to 10.6 μg/kg, and the limits of quantification（LOQs） of the tested pesticides were between 2.1 and 35.5 μg/kg.（2） In the linear range between 1 μg/L and 950 μg/L of each pesticide, the linear correlation coefficients were between 0.9956 and 1.0000.（3）At the spiked levels of 7.3 to 620 μg/kg in the wheat extract,the average recoveries ranged from 66.6 % to 118.2 % and the relative standard deviations（RSDs） were between 1.0 % and 18.0 %.（4）The method covered a wide range of pesticides with the advantages of simple and rapid pretreatment, saving solvent and capable of analyzing 109 pesticides accurately and sensitively by a single sample injection.

关 键 词：程序升温汽化-气相色谱-三重四极杆串联质谱 小麦 农药残留 

分 类 号：O657.63[理学—分析化学] TS210.7[理学—化学]