柱后衍生-高效液相色谱-荧光检测法测定土壤中氨基甲酸酯农药

Determination of carbamate pesticide residues in soil by Post-column Derivatization-HPLC with Fluorescence Detection

目的建立柱后衍生一高效液相色谱一荧光检测法测定土壤中7种氨基甲酸酯类农药残留的方法。方法土壤样品经初筛后用乙腈一氯化钠萃取,用丙酮及二氯甲烷(1:1)混合溶剂作淋洗剂,经过Florisil SPE柱纯化,淋出液经氮吹蒸近干后用甲醇溶解,所得溶液用柱后衍生-高效液相色谱-荧光检测法进行定性及定量分析。结果此方法的检出限在0.001 mg/kkg-0.01 mgkg之间,回收率和相对标准偏差(RSD)范围分别为88.80%-101.10%和1.30%-6.10%。结论所建立的方法符合方法学要求并可应用于土壤环境监测工作。

objectives To establish a method for detecting seven carbamate pesticide residues in soil by Post columnDerivatization HPLC with Fluorescence Detection. Methods The carbamate pesticides were extracted from soilusing acetonitrile as extracting solvent. Using acetone and dichloromethane （ 1 ： 1 ） as the eluent, we passed the solutionthough Florisil SPE column purification. The leaching solution was almost evaporated to dry by blowing nitrogen anddissolved in methanol.Finally, the extracted pesticide residues were analyzed by Post column Derivatization HPLC withFluorescence Detection for qualitative analysis and quantitative analysis. Results the lowest determination limit of thismethod was 0.008 mg/kg or better, the rate of recovery was 88.8% -101.1% and relative standard deviation （RSD） as1.3%-6.1%. Conclusion This method conforms to requirement of the concerned standard, and meets theenvironmental monitoring needs.