【目的】建立吡蚜酮、氧乐果、敌百虫、啶虫脒、乐果、甲磺隆、氯磺隆、多效唑、嘧菌环胺、烯唑醇、喹硫磷、甲氨基阿维菌素苯甲酸盐12种农药在小麦中的液相色谱-三重串联质谱同时检测和确证方法。【方法】小麦样品经粉碎后,0.1%(体积分数)冰醋酸-乙腈提取,NH:氨基柱填料和石墨化炭黑固相分散净化,含0.1%甲酸的乙腈水混合液定容过微孔滤膜后用液相色谱串联四级杆质谱联用仪LC—MS—MS检测和确证。【结果】方法在10—1000gg/L范围内保持良好的线性关系,相关系数大于0.99。12种农药在10、50、100μg/kg添加水平的回收率和相对标准偏差的数据表明:12种农药的回收率均为72%-107%,RSD为1.5%-13.3%,回收率和相对标准偏差达到相应标准的要求。【结论】该方法快速、灵敏、适用广泛、操作简便及污染小,适用于小麦籽粒中农药残留的定性定量分析。
[Aims] The LC-MS-MS (liquid chromatography tandem triple quadrupole mass spectrometry) method for determination of twelve pesticides (pymetrozine, omethoate, trichlorphon, acetamiprid, dimethoate, metsulfuronmethyl, chlorsulfuron, paclobutrazol, cyprodinil, diniconazole, quinalphos, emamectin-benzoate) was developed. [Methods] Wheat samples were extracted with 0.1% HAc-actonitrile after smashed, then the extraction was cleaned by NH2 and graphite carbon. The solution was filtered with a membrane before injected into the instrument. [Results] For the above method, the linear scope was 10-1000 μg/L. Linear correlation coefficients was over 0.99. The range of the recoveries was 72-107%, the range of RSD was 1.5-13.3%, in the three levels of 10, 50, 100 μg/kg for 12 pesticides. [Conclusions] These results showed that the method was fast, sensitive, convenient and widely available with less pollution and suitable for the determination of pesticides in wheat.