分子印迹固相萃取-高效液相色谱法测定植物油中多环芳烃

Determination of polycyclic aromatic hydrocarbons in vegetable oil by molecular imprinting solid-phase extraction-high performance liquid chromatography

中文关键词:  高效液相色谱  植物油  分子印迹  固相萃取  多环芳烃

英文关键词:high performance liquid chromatography  vegetable oil  molecularly imprinted  solid phase extraction  polycyclic aromatic hydrocarbons

中文摘要:

      目的 建立植物油中多环芳烃的分子印迹固相萃取-高效液相色谱快速测定方法。方法 采用正己烷溶解植物油样品, 将样品上样于活化和平衡后的分子印迹固相萃取小柱, 正己烷淋洗, 二氯甲烷洗脱, 氮吹至近干后, 1 mL正己烷定容, 0.22 μm亲水系PTFE滤膜过滤, 高效液相色谱法荧光检测器测定, 保留时间定性, 色谱峰面积定量。结果 多环芳烃在1~100 ng/mL浓度范围内, 峰面积呈良好线性, 线性相关系数均达到0.999以上。多环芳烃在5.0、20.0、50.0 μg/kg 3个不同添加水平的回收率为76.0%~103.6%, 相对标准偏差(relative standard deviation, RSD)均小于10%。结论 该方法具有简便、快速、灵敏高、准确度好等优点, 可满足植物油中多环芳烃的定量分析。

英文摘要:

      Objective To establish a method for rapid determination of polycyclic aromatic hydrocarbons in vegetable oils by molecular imprinting solid-phase extraction-high performance liquid chromatography. Methods Samples were dissolved with n-hexane. The disposed samples were transferred to activated and balanced molecularly imprinted solid phase extraction micro-columns, washed with n-hexane, eluated with dichloromethane, dried with nitrogen, dissolved with 1 mL acetonitrile, and screened with 0.22 μm pro-drainage PTFE filtration membrane. Then, they were detected by high performance liquid chromatography with fluorescence detector, qualitatively analyzed with retention time, and quantitatively analyzed with peak area, respectively. Results Polycyclic aromatic hydrocarbons showed a good linear relationship in the range of 1-100 ng/mL, and correlation coefficients were all above 0.999. The recoveries of polycyclic aromatic hydrocarbons at 3 spiked levels (5.0, 20.0, 50.0 μg/kg) were 76.0%-103.6%, with the relative standard deviations all below 10%. Conclusion This method is simple, rapid, sensitive and accurate, which can satisfy the quantitative analysis of polycyclic aromatic hydrocarbons in vegetable oils.