QuEChERS-GC-MS/MS法同时测定竹笋中49种农药残留量  

Determination of 49 Pesticides Residues in Bamboo Shoot Using QuEChERS-modified and Gas Chromatography-tandem Mass Spectrometry

作　　者：褚能明[1,2] 杨俊英[1,2] 柴勇[1,2] 康月琼[1,2] 张雪梅[1,2] 

机构地区：[1]重庆市农业科学院农业质量标准与检测技术研究所,重庆401329 [2]农业部农产品质量监督检验测试中心(重庆),重庆401329

出　　处：《西南农业学报》2015年第3期1288-1294,共7页Southwest China Journal of Agricultural Sciences

基　　金：重庆市科委项目特色农作物典型污染本底值检测与农产品质量安全评价(cstc2013yykf8002-12)

摘　　要：以优化改进的QuEChERS方法为基础,建立了利用气相串联质谱法（GC-MS/MS）同时测定竹笋中49种农药残留量的方法。样品用乙腈提取、盐析分层后,经PSA和C18两种混合固相吸附剂净化,最后用甲苯溶解样品上机检测。49种农药的响应值与其质量浓度线性关系良好,相关系数在0.99以上,检出限范围为1.0~26.2μg/kg。在添加水平分别为10.0,50.0和100.0μg/kg时,除百菌清在添加水平为10.0μg/kg添加回收率为58.6%外,其余各农药的回收率在62.5%~121.8%之间,相对标准偏差为0.8%~11.7%,符合农药残留分析要求,可以用于竹笋中农药残留的监测。A mixture of 49 pesticides amenable to gas chromatography （GC） were quantitatively recovered from spiked bamboo shoot, based on QuEChEBS-medified, and determined using gas chromatography-tandem mass spectrometry （C,C-MS/MS）. The method employed in- volved initial extraction in a acetonitrile, an extraction/partitioning step after the addition of salt, and a cleanup step utilizing dispersive sol- id-phase extraction by PSA and C18. The sample was dissolved in toluene, and then determined by GC-MS/MS. This combination ensured that it was a rapid, simple and cost-effeetive procedure. For 49 pesticides, the LOD ranged horn 1.0 to 26.2μg/kg respectively, the cone- lation coefficient was above 0. 99. The spiking levels for the recovery experiments were 10.0, 50. 0 and 100.0 μg/ kg for C,C-MS/MS analy- ses. Mean recoveries mostly ranged between 62.5 % and 121.8 % and relative standant deviations （RSD） were generally 0.8 % - 11.7 %. Based on these results, the methodology has been proved to be highly efficient and robust and thus suitable for monitoring the pesticide residue in bamboo shoot.

关 键 词：QU ECh ERS方法 气相串联质谱法(GC-MS/MS) 竹笋 农药残留 

分 类 号：S481.8[农业科学—农药学]