凝胶渗透色谱-高效液相色谱法测定蔬菜中呋喃丹的含量

Determination of carbofuran in vegetables by gel permeation chromatography-highperformance liquid chromatography

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 method for determination of carbofuraninvegetablesby high performance liquid chromatography（HPLC） with purification ofgel permeation chromatography（GPC）.Methods Samples were extracted withacetonitrile and dissolved with ethyl acetate-cyclohexanemixture,and then separated by reversed-phase C_（18）column followed with GPC purification.The fluorescence excitation and emission wavelengths were 285 nm and320 nm.Identification of carbofuran was performed by HPLC with an external standard method.Results Carbofuranhad a good linear relationship in the range of 0.2~5.0 ng/mL with the correlation coefficient greater than0.999.The limit of detection（LOD） was0.01mg/kg.The average recoveries at 3 spiked levels of 0.5,1.0 and 2.0mg/kg were ranged from 78.3%to 97.6%,and the relative standard deviations（RSD）were in the range of3.26%~11.69%.Conclusion The established method is simple and sensitive,which issuitable forthe determination of carbofuran in vegetables.