甘蔗中杀螟丹农药残留前处理方法的优化及检测

摘要

The extraction ratio of cartap residual under two different acidic solutions, the efficiency of cartap convert into nereistoxin under two different basicity and catalyst conditions, and the extraction efficiency of three extract agent on nereistoxin, were investigated. The pretreatment method for cartap residues in sugarcane was optimized. Applied column DB-35(30.0 m×320 μm×0.25μm), program warming, FPD-S and ECD as detection, the recovery rate of FPD-S was 87%~102%, RSD was 8.0%, there was a good linear relationship between 0.01~0.10mg/L, r=0.9988, the method detection limit was 0.3μg/kg; the recovery rate of ECD was 84%~93%, RSD was 7.3%, there was also a good linear relationship between 0.01~0.10mg/L, r=0.9966, and the method detection limit was 0.1μg/kg.%考察了两种不同酸性溶液对甘蔗中杀螟丹残留的提取率,两种不同的碱性及催化剂条件下杀螟丹转化成沙蚕毒素的转化率,以及3种提取剂对沙蚕毒素的提取效率,优化了甘蔗中杀螟丹农药残留的前处理方法.以DB-35 (30.0m×320μm×0.25μm) 色谱柱分离,程序升温,分别采用具硫滤光片的火焰光度检测器(FPD-S)和电子俘获检测器(ECD)进行检测.其中FPD-S方法的添加回收率为87%~102%,相对标准偏差(RSD)为8.0%,在0.01~0.10 mg·L-1之间具有良好的线性关系,r=0.9988,方法检出限为0.3μg·kg-1.ECD方法的添加回收率为84%~93%,相对标准偏差(RSD)为7.3%,在0.01~0.10 mg·L-1之间具有良好的线性关系,r=0.9996,方法检出限为0.1μg·kg-1.建立的杀螟丹检测方法,前处理简单,方法准确,重现性好,满足农药残留检测的要求.