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目的建立凝胶渗透色谱-高效液相色谱法检测蔬菜中的呋喃丹农药残留量。方法样品经乙腈提取和环己烷-乙酸乙酯溶解后,经凝胶渗透色谱净化和反相高效液相C_(18)色谱柱分离后,采用荧光检测器进行测定,荧光检测激发波长为285 nm,发射波长为320 nm,采用高效液相色谱法以外标法定量。结果呋喃丹在0.2~5.0 ng/mL浓度范围内呈良好线性关系,相关系数r大于0.999,检测限为0.01 mg/kg。对空白蔬菜样品进行呋喃丹3个浓度水平0.5、1.0和2.0 mg/kg的加标,回收率结果为78.3%~97.6%,相对标准偏差为3.26%~11.69%。结论本研究所建立的方法简单、灵敏度高,可适用于蔬菜中的呋喃丹农药残留的分析检测。
Objective To establish a gel permeation chromatography - high performance liquid chromatographic method for the determination of carbofuran pesticide residues in vegetables. Methods After the sample was extracted by acetonitrile and dissolved in cyclohexane - ethyl acetate, the sample was separated by gel permeation chromatography and reverse phase high performance liquid chromatography on a C 18 column. The fluorescence detector was used to detect the excitation wavelength of 285 nm, the emission wavelength of 320 nm, using high performance liquid chromatography to external standard method. Results There was a good linear relationship between the concentration of carbofuran and 0.2 ~ 5.0 ng / mL. The correlation coefficient r was greater than 0.999 and the limit of detection was 0.01 mg / kg. The blank vegetable samples were spiked at concentrations of 0.5, 1.0 and 2.0 mg / kg of furadan at 78.3% -97.6% with relative standard deviations of 3.26% ~ 11.69%. Conclusion The method established in this study is simple and sensitive and can be applied to the analysis and detection of carbofuran residues in vegetables.