磁分散萃取结合气质谱联用法同时测定植物油中24种多环芳烃

Simultaneous determination of 24 polycyclic aromatic hydrocarbons in vegetable oils using magnetic dispersive solid-phase extraction combined with gas chromatography-mass spectrometry

目的建立一种快速、高效、准确的测定植物油中24种多环芳烃(PAHs)的磁分散固相萃取-气相色谱质谱联用法。方法以自制的氨基功能化磁性碳纳米管(EDA-@Mag-CNTs)为吸附剂,经磁分散固相萃取进行富集,经甲苯洗脱后采用DB-EUPA毛细管柱和质谱检测器对植物油中多环芳烃进行检测,同位素内标法定量。结果 24种多环芳烃在1μg/L～250μg/L有很好的相关性,相关系数均> 0. 998 5,该方法最低检出限为0. 1μg/kg～1. 0μg/kg,最低定量限为0. 3μg/kg～3. 0μg/kg;在低、高2种加标水平下,回收率分别为83. 2%～96. 6%和85. 2%～98. 9%。结论本方法操作简便、快速、灵敏度高,可用于植物油中24种多环芳烃的检测。通过对27份植物油样品的测定,初步得到衢州市售植物油中多环芳烃的污染特征,通过植物油摄入多环芳烃的健康风险需引起关注。

Objective To develop a rapid,effective and accurate method for the determination of 24 polycyclic aromatic hydrocarbons(PAHs)in vegetable oils by magnetic dispersive solid-phase extraction combined with gas chromatography and mass spectrometry (MSPE-GC/MS).Methods The target PAHs were enriched,ethylenediamine -functionalized magnetic carbon nanotubes(EDA -@Mag-CNTs),by magnetic dispersion solid phase extraction,and eluted with toluene;the polyeyclic aromatic hydrocarbons in vegetable oil were detected by DB -EUPA capillary column and mass spectrometer,and quantified by isotope internal standard method.Results The 24 kinds of PAHs showed good linearity in the range of 1μg/L -250μg/L (r >0.9985).The limits of detection(LODs)in vegetable oils of 24 PAHs were witin 0.1μg/kg-1.0μg/kg and the limits of quantification(LOQs)were within 0.3μg/kg -3.0μg/kg.Recoveries were within 83.2%-96.6% at low spiked level, and 85.2%-98.9% at high spiked level.Conclusion The developed method is simple,rapid and sensitive,and can be applied to the analysis of 24 PAHs in vegetable oils.The pollution characteristics in vegetable oil in Quzhou was preliminarily acquired by the determination of 27 samples.So,the health risks by PAHs intake from vegetable oil should be concerned.