超高效液相色谱法同时测定植物油中15种多环芳烃类添加剂

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

作者信息

Dong Guixian, Wang Zhaoxia, Zhou Xiaoge, Zhang Xiaoyu, Wang Ying, Zhang Guifang

出版信息

Wei Sheng Yan Jiu. 2014 Jul;43(4):620-3.

PMID:25199292

Abstract

OBJECTIVE

To establish a rapid method for simultaneous determination of 15 polycyclic 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 C18 (4.6 mm x 250 mm, 3 microm) 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 degrees C, and the injection was 10 microl. 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 microg/L, the peak area and content was in a good linear relationship (r > or = 0.9990). The average recoveries of three spiked levels (10, 50 and 100 microg/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 microg/kg and the limits of quantification were 0.08 - 3.0 microg/kg.

CONCLUSION

This method is simple and quick with high sensitivity, and it is suitable for the determination of 15 PAHs in vegetable oil.

摘要

目的

建立超高效液相色谱-荧光检测法同时测定植物油中15种多环芳烃（PAHs）的快速方法。

方法

植物油用乙腈和丙酮（1∶1）提取，经Oasis HLB柱和Sep-Pak弗罗里硅土柱净化，采用Waters PAH C18（4.6 mm×250 mm，3μm）多环芳烃分析专用柱，以乙腈、甲醇和水为流动相进行梯度洗脱，柱温35℃，进样量10μl。用荧光检测器测定样品中PAHs的浓度，外标法定量。

结果

15种PAHs在9 min内完全分离。在2～200μg/L范围内，峰面积与含量呈良好的线性关系（r≥0.9990）。3个加标水平（10、50和100μg/kg）的平均回收率为75.8%～96.4%，相对标准偏差为3.42%～8.03%（n = 5）。检出限为0.025～0.8μg/kg，定量限为0.08～3.0μg/kg。