分散固相萃取--高效液相色谱检测花生中咪唑乙烟酸残留

摘要

A method was developed for the determination of the imazethapyr residue in peanut by using QuEChERS and HPLC-UVD.The imazethapyr residue in peanut sample was vortex extracted by the methanol and purified by PSA,and than analyzed by using HPLC-UVD with Agilent ZORBAX Extend-C18 column.The chromatographic conditions of analysis were critically optimized and the results showed good linearity in the ranges from 0.05 to 10.0 mg/L (y=4.003 8x-0.275 6,R2=0.999 5).The detection limit of the method was 0.016 mg/L.And the average recoveries of imazethapyr in peanut samples were all above 85% at three spiking levels of 0.05,0.1 and 0.5 mg/kg with relative standard deviations all under 10%.Limit of quantification of imazethapyr in peanut was 0.036 mg/kg.The method is simple,economic,efficient and sensitive,and it is suitable for the determination of imazethapyr residues in peanut.%确立了花生籽粒样品中咪唑乙烟酸残留的甲醇涡旋提取、PSA净化的分散固相萃取样品前处理程序,建立并优化了高效液相色谱样品检测方法.结果显示：在确定的色谱条件下,咪唑乙烟酸在0.05~10.0 mg/L质量浓度范围内与对应的色谱峰面积线性响应良好,其回归方程为y=4.0038x-0.2756（R2=0.9995）,方法的检出限（LOD）为0.016 mg/L.咪唑乙烟酸0.05、0.10和0.50 mg/kg 3个添加水平的平均回收率均在85%以上,RSD均小于10%,方法的检测限（LOQ）为0.036 mg/kg.表明所建立残留样品前处理方法和高效液相色谱检测方法简便、经济、快速、灵敏,适于花生中咪唑乙烟酸残留量的检测.