建立了超高效液相色谱-串联质谱法(UPLC-MS/MS),可于10 min内快速测定土壤中的239种农药残留.土壤样品经AOAC (Association of Official Analytical Chemists) QuEChERS方法处理,用乙腈萃取;无水硫酸镁、乙酸钠固液分离后,过0.2μm滤膜;在UPLC-MS/MS正、负离子同步扫描多反应监测模式下进行分析.239种农药中,线性相关系数(r2)大于0.99的有236个,占总数的99%.在40 μg/kg添加水平下所有被检测农药的回收率均在50% ~ 150%之间,且相对标准偏差(RSD)均小于20%;其中有209种农药的回收率达到70% ~ 120%,有161种的RSD小于10%.方法的检出限(LOD)范围为0.69 ~ 29.04 μg/kg.土壤中多种农药残留的同时检测要求时间短、准确度和精密度高,本方法符合这些检测要求,适用于土壤中农药残留的检测.
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