联苯肼酯在柑橘及其土壤中的残留分析方法

Residue analysis of bifenazate in citrus and soil

摘要: 采用高效液相色谱仪建立了联苯肼酯在柑橘及土壤中的残留分析方法。柑橘样品采用V(乙腈):V(乙酸乙酯)=1:1、土壤样品采用V(丙酮):V(二硫化碳)=1:1的混合溶剂超声提取,碱性氧化铝柱层析净化,高效液相色谱-二极管阵列检测器(HPLC-DAD)测定。在0.05～10 mg/L范围内联苯肼酯峰面积与进样质量浓度呈良好线性关系,R2=0.999 4。该方法的定量限为0.02 mg/kg。在0.02～1 mg/kg添加水平下,联苯肼酯的添加回收率为80.47%～98.93%,相对标准偏差为2.62%～7.32%。方法的精确度、灵敏度和稳定性均符合农药残留分析的要求。

Abstract: The high performance liquid chromatographic method was described for the determination of bifenazate in citrus and soil.The citrus samples were ultrasonic-extracted with hexane-ethyl acetate and cleaned up by Alkali alumina,the soil samples were ultrasonic-extracted with carbon disulfide-acetone,and then detected by HPLC-DAD.The linear relationship of bifenazate was found better in the concentration range from 0.05 to 10.00 μg/mL with the linear correlation of 0.999 4.In the present method,the lowest limit of quantification was 0.02 mg/kg. The average recovery varied from 87.12% to 98.93%,and the RSD ranged from 2.62% to 7.32%at the addition level of 0.02-1 mg/kg.The method accuracy,sensitivity and stability are in line with the requirement of pesticide residue analysis.