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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0.05~5 mg/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=10 243x+233.0(R~2=0.999 0);土壤和柑橘中环氧虫啶的最低检测浓度均为0.1 mg/kg;在0.1~1 mg/kg 3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。
A high performance liquid chromatography (HPLC-UVD) method was developed for the determination of residual pesticides in citrus and soil. Citrus samples were extracted with V (distilled water): V (dichloromethane) = 1: 2 and purified by Florisil column (determined directly after extraction of soil samples), HPLC-UVD assay and external standard method, Methods The field samples were tested for the determination of epoxide. The results showed that the linear equation was y = 10 243x + 233.0 (R ~ 2 = 0.999 0) in the range of 0.05-5 mg / L, and the linear relationship between the mass concentration of epoxy and the corresponding peak area was linear. The lowest detectable concentration of epicotoxin in citrus was 0.1 mg / kg. The average recovery of ephedrine in soil and citrus was between 76% and 93% at the three levels of 0.1-1 mg / kg The relative standard deviations (RSD, n = 5) ranged from 1.6% to 5.8%. The method is rapid, sensitive and stable and can be used for the determination of epicotofenac residues in citrus and soil.