高效液相色谱法检测环氧虫啶在柑橘及土壤中的残留

建立了环氧虫啶在柑橘和土壤中残留量测定的高效液相色谱(HPLC-UVD)分析方法。柑橘样品采用V(蒸馏水):V(二氯甲烷)=1:2提取后经弗罗里硅土柱净化(土壤样品提取后直接测定),HPLC-UVD测定,外标法定量,并运用此方法对田间样品进行了环氧虫啶残留量检测验证。结果表明:在0.05~5mg/L范围内,环氧虫啶质量浓度与对应的峰面积间呈良好线性关系,线性方程为y=10243x+233.0(R2=0.9990);土壤和柑橘中环氧虫啶的最低检测浓度均为0.1mg/kg;在0.1~1mg/kg3个添加水平下,环氧虫啶在土壤和柑橘中的平均回收率在76%~93%之间,相对标准偏差(RSD,n=5)在1.6%~5.8%之间。该方法快速、灵敏、稳定,可用于柑橘和土壤中环氧虫啶残留量的检测。

Determination of cycloxaprid in citrus and soil by high performance liquid chromatography

A high performance liquid chromatography (HPLC-UVD) method was established for the analysis of cycloxaprid residues in citrus and soil. Citrus samples were extracted with dichloromethanedistillate (2:1, V/V) and cleaned up by Florisil adsorption column and detected by HPLC-UVD. And soil samples was detected directly after the extraction. The external standard method was adopted for the quantification. This analytical method was used to determine the cycloxaprid residue in field samples. The results showed that there was a good linear relationship between the target substance concentration and the peak area in the range of 0.05-5 mg/L, The linear equation was y = 10 243x + 233.0 (R² = 0.999 0), and the minimum detectable concentration in citrus and soil was both 0.1 mg/kg. The average recoveries in citrus and soil were from 76% to 93% at the fortified level of 0.1 mg/kg to 1 mg/kg, and the relative standard deviation (RSD, n = 5) was between 1.6% to 5.8%. The detection method was rapid, sensitive and stable. Thus it could be applied to determine cycloxaprid residues in soil and citrus.