高效液相色谱法测定蔬菜和土壤中氯虫苯甲酰胺甲氧虫酰肼的残留

Study on Chlorantraniliprole and Methoxyfenozide Residue in Vegetables and Soil by HPLC

建立了同时测定蔬菜(黄瓜、青菜、豇豆、卷心菜、番茄)、土壤中氯虫苯甲酰胺和甲氧虫酰肼农药残留的高效液相色谱法。蔬菜以乙腈高速匀浆提取,过NH2小柱净化,再用甲醇定容。而土壤样品较干净,经乙腈振荡提取1h,浓缩后定容过膜即可。采用甲醇–乙腈–水为流动相,利用C18柱和紫外检测器(检测波长:230nm)对待测组分进行了分离和测定。实验证明,添加浓度在0.05mg/kg、0.4mg/kg和1mg/kg时,蔬菜和土壤中氯虫苯甲酰胺和甲氧虫酰肼平均添加回收率在87.6%～114.4%之间,相对标准偏差(RSD)<10%,氯虫苯甲酰胺和甲氧虫酰肼在样品中的最低检出浓度为0.05mg/kg,最小检出量为1ng。

A high performance liquid chromatography （HPLC） method was developed for the determination of chlorantraniliprole and methoxyfenozide in vegetables （cucumber,greengrocery,cowpea,cabbage and tomato） and soil. The residues of vegetable and soil samples were extracted with acetonitrile,and vegetable samples were cleaned up with NH2 Solid-phase extraction,and condensed to dry. Determinations of analytes were completed using HPLC with DAD detection at 230 nm. Under HPLC conditions,The fortified recoveries of phenazine-1-carboxylic acid in straw,chaff and unpolished grain were in range of 87.6%-114.4%,with relative standard deviations less than 10%. and the minimum determination concentration was 0.05 mg/kg in these samples,the detectable limit of chlorantraniliprole and methoxyfenozide was estimated to be 1 ng.