超高效液相色谱法同时测定植物油中15种多环芳烃

Simultaneous determination of 15 polycyclic aromatic hydrocarbons additives in vegetable oil by ultra performance liquid chromatography

目的建立采用超高效液相色谱（UPLC）-荧光检测器（FLR）同时快速检测植物油中15种多环芳烃的方法。方法采用乙腈：丙酮（1：1）混合溶剂提取，先后使用Waters的OasisHLB和Sep-PakFlorsil小柱净化，WatersPAHC18色谱柱（4．6mm×50mill，3恤m）分离，甲醇、乙腈和水进行梯度洗脱，柱温35℃，流速0．80ml／min，进样量10μ1；荧光检测器采用程序定时控制荧光检测波长变化，外标法定量。结果15种多环芳烃9min内完全分离，在2．0～200．0μg／L范围内，峰面积和质量浓度的线性关系良好（r≥0．9990），以高、中、低浓度（10、50和100μg／kg）作为不同的添加水平，平均加标回收率为75．8％～96．4％，RSD为3．42％～8．03％（12=5），检出限为0．025～0．8μg／kg，定量限为0．08，3．0μg／kg。结论该方法操作方便、分离效果好、线性范围宽，能满足植物油中15种多环芳烃的检测要求。

Objective To establish a rapid method for simultaneous determination of 15polycyclic aromatic hydrocarbons （PAHs）in vegetable oil by ultra performance liquid chromatography with fluorescence detection. Methods The vegetable oils were extracted with acetonitrile and acetone （ 1 ： 1 ） , purified with Oasis HLB and Sep-Pak Florsil column, separated on Waters PAH C1s （4.6 mm × 250 mm,3 μm） special column for the analysis of polycyclic aromatic hydrocarbons with a mobile phase of acetonitrile, methanol and water for gradient elution,the column temperature was 35 ℃ , and the injection was 10 μl. The concentration of PAHs in samples were determined with fluorescence detector, and quantitative analysis was carried out by external standard. Results The 15 PAHs were completely separated within 9 min. Within 2 to 200 μg/L,the peak area and content was （10 good linear relationship （r≥0. 9990）. The average recoveries of three spiked levels 50 and 100μg/kg） were 75.8% and 96.4% ,with RSDs of 3.42% -8.03%（n= 5）. The limits of detection were 0. 025 - 0. 8 μg/kg and the limits of quantification were 0.08 -3.0 μg/kg. Conclusion This method is simple and quick with high sensitivity, and it is suitable for the determination of 15 PAHs in vegetable oil.