高效液相色谱法检测环氧虫啶在柑橘及土壤中的残留  

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

作　　者：聂红英[1,2] 杨仁斌[1] 赵运林[2] 吴育佳[3] 欧阳文森[2] 

机构地区：[1]湖南农业大学农业环境保护研究所,长沙410128 [2]湖南农业大学生物科学技术学院,长沙410128 [3]杭州师范大学生命环境与科学学院,杭州310036

出　　处：《农药学学报》2016年第3期352-357,共6页Chinese Journal of Pesticide Science

基　　金：农业部农药登记残留项目(2013P295)

摘　　要：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 established for the analysis of cycloxaprid residues in citrus and soil. Citrus samples were extracted with dichloromethane- distillate （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.

关 键 词：高效液相色谱 环氧虫啶 柑橘 土壤 残留 

分 类 号：S482.3[农业科学—农药学] O657.72[农业科学—植物保护]