凝胶渗透色谱-高效液相色谱法测定蔬菜中 呋喃丹的含量

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。

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

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 C18column followed with GPC purification.The fluorescence excitation and emission wavelengths were 285 nm and 320 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 than 0.999. The limit of detection(LOD) was0.01mg/kg. The average recoveries at 3 spiked levels of 0.5, 1.0 and 2.0 mg/kg were ranged from 78.3% to 97.6%, and the relative standard deviations(RSD)were in the range of 3.26%~11.69%. Conclusion The established method is simple and sensitive, which issuitable forthe determination of carbofuran in vegetables.