高效液相色谱-二极管阵列检测器-荧光检测器法测定植物油中的18种多环芳烃

Determination of 18 Polycyclic Aromatic Hydrocarbons in Vegetable Oil by High Performance Liquid Chromatography with Diodearry Detector and Fluorescence Detector

建立凝胶渗透色谱法净化样品、高效液相色谱-二极管阵列串联荧光检测器法同时测定植物油中18种多环芳烃的检测方法。样品经环己烷-乙酸乙酯（1：1，V／V）溶解，利用凝胶渗透色谱法去除油脂大分子，PAHC18柱分离，乙腈和水作流动相进行梯度洗脱，设置荧光检测程序，以2个发射波长通道同时采集数据，测定油样中的17种多环芳烃，以二极管阵列检测器测定苊烯。结果表明：方法检出限为0．5-4ng／mL，样品回收率在78．65％-103-4％之间，相对标准偏差小于5％。本方法满足德国标准对18种多环芳烃的同步检测新要求。

A method has been developed for the simultaneous determination of 18 polycyclic aromatic hydrocarbons in vegetable oil by gel permeation chromatography （GPC） and high performance liquid chromatography with diodearray detector and fluorescence detector （HPLC-DAD-FLD）. The samples were dissolved in cyclohexane-ethyl acetate （1：1, V/V）, then purified with GPC to remove grease molecules, and separated on a PAH C18 column using acetonitrile and water as the mobile phase with gradient elution. Subjected to 2-wavelength channel data acquisition setting with fluorescence procedure, 17 kinds of polycyclic aromatic hydrocarbons in oil samples were determined. Data acquisition of acenaphthylene was achieved by DAD detector. The detection limit of this method was 0.5-4 ng/mL. The average recovery rate in oil was in the range of 78.65%-103.4% with relative standard deviation （RSD） of less than 5%, This method was satisfactorily used for the simultaneous detection of 18 kinds of polycyclic aromatic hydrocarbons （PAHs） in edible oil, while meeting the new detection requirements of Germany standards for these PAHs.