甘蔗中杀虫双农药残留前处理方法优化及检测

Optimization and detection of bisultap residues in sugarcane

考察2种不同酸性溶液对甘蔗中杀虫双残留提取率,2种不同碱性及催化剂条件下杀虫双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,优化甘蔗中杀虫双农药残留前处理方法。以DB-35(30.0 m×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方法添加回收率为80%~89%,相对标准偏差(RSD)为5.1%,在(0.01~0.10)mg/L之间具有良好的线性关系,R=0.9979,方法检出限为0.3μg/kg。ECD方法添加回收率为80%~87%,相对标准偏差(RSD)为8.4%,在(0.01~0.10)mg/L之间具有良好的线性关系,R=0.9986,方法检出限为0.1μg/kg。建立的杀虫双检测方法,前处理简单、方法准确、重现性好,满足农药残留检测的要求。

Two different acidic solutions as the extraction, two different basicity and catalyst conditions as the conversion and the three extracts were investigated in this method. Optimization the pretreatment method for bisultap residues in sugarcane. Column DB-35 （30.0 mx320 pmx0.25 pm）, Program warming, FPD-S and ECD as detection. For FPD-S the recovery rate was 80%-89%, RSD 5.1%, there was a good linear relationship between （0.01-0.10）mg/L, R=0.9979, and the method detection limit was 0.3 pg/kg. For ECD the recovery rate was 80%-87%, RSD 8.4%, there was also a good linear relationship between （0.01-0.10）mg/L, R=0.9986, and the method detection limit was 0.1 pg/kg. The method was simple, accurate and good reproducible to meet the requirement of pesticide residue detection.