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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 temperature-programmed vaporization-gas chromatography-triple quadrupole mass spectrometry (PTV-GC-MS / MS) method was developed for the simultaneous determination of 109 pesticide residues (121 components) in wheat. The wheat samples were rapidly extracted and purified by Qu ECh ERS technique. After PTV injection, they were separated on the capillary column TR-Pesticide II. The retention time window and the characteristic SRM (selective reaction monitoring) ion pairs were used for qualitative and peak area quantification. The results showed that: (1) The limit of detection (LOD) of 109 pesticides was 0.6 ~ 10.6μg / kg in wheat and LOQ was 2.1 ~ 35.5μg / kg; (2) (3) The average recoveries ranged from 66.6% to 118.2% and the RSD ranged from 1.0% to 18.0% when the concentration was between 7.3 and 620 μg / kg in wheat samples. 4) The method covers a wide range of pesticide varieties, pre-treatment is simple and fast, solvent-saving, one injection can analyze 109 kinds of pesticides, accurate and sensitive.