全自动分子印迹固相萃取高效液相色谱法测定 食用油中10种多环芳烃Determination of ten polycyclic aromatic hydrocarbons in edible oil by using fully automatic molecularly imprinted solid phase extraction coupled with high performance liquid chromatography

Abstract

为快速测定食用油中的多环芳烃，建立全自动分子印迹固相萃取高效液相色谱法测定食用油中10种多环芳烃的分析方法。将样品用正己烷溶解，以2 mL正己烷为淋洗液，二氯甲烷为洗脱剂，经全自动分子印迹固相萃取柱净化，氮吹后定容进高效液相色谱仪（配荧光检测器）检测。结果表明：所建方法线性关系良好，检出限为0.1~1.3 μg/kg，定量限为0.3~4.0 μg/kg；方法的准确度良好，精密度高，10种多环芳烃在玉米油和花生油基质中的加标回收率为79.2%~114.3%，相对标准偏差为0.4%~5.7%，将该方法应用于实际食用油样品中苯并［a］芘的测定，所测样品中苯并［a］芘含量均未超出国标限量。所建方法前处理简单快速，可实现固相萃取柱的自动化处理，减少有机溶剂的消耗，适合食用油中多环芳烃的快速测定。 For rapid determination of polycyclic aromatic hydrocarbons(PAHs)in edible oil, an analysis method for the determination of 10 PAHs in edible oil by using fully automatic molecularly imprinted solid phase extraction and high performance liquid chromatography (HPLC) was established. The sample was dissolved in n-hexane, purified by a molecularly imprinted solid phase extraction column, with 2 mL n-hexane as leaching solution, dichloromethane as elution solvent, and detected by HPLC with fluorescence detector after evaporated by nitrogen. The results showed that the method had a good linear relationship, and high accuracy and good precision. The limit of detection was 0.1-1.3 μg/kg, and the limit of quantitation was 0.3-4.0 μg/kg. The recovery of 10 PAHs in corn oil and peanut oil was 79.2%-114.3% with RSD 0.4%-5.7%. Applying the method to the determination of BaP in actual edible oil samples, the results showed that the BaP in the oils didn′t exceed the national standard limit. The pretreatment is simple and fast, which can realize the automatic processing of solid phase extraction columns and reduce the consumption of solvents. The method established is suitable for the rapid determination of PAHs in edible oil.

Keywords

• 固相萃取；分子印迹；多环芳烃；食用油；高效液相色谱
• solid phase extraction; molecular imprinting; polycyclic aromatic hydrocarbons; edible oil; high performance liquid chromatography