【摘要】 目的建立一种分子印记固相萃取-气相色谱/质谱联用(MISPE-GC/MS)法测定食用油中16种多环芳烃(PAHs)的检测方法。方法样品经正己烷稀释后,于高分子印记固相萃取柱净化,正己烷淋洗除杂,二氯甲烷洗脱,洗脱液最终浓缩定容至200μL,采用气相色谱毛细管柱(30 m×0.25 mm×0.25μm)分离,选择离子模式进行扫描,同位素内标法定量。结果 16种多环芳烃在2~20μg/L范围内有很好的相关性,相关系数均大于0.998;检出限范围为0.1~0.6μg/kg;在2μg/kg和10μg/kg两个加标水平下,加标回收率范围为75.5%~125.2%(n=6),相对标准偏差均小于15%。结论 MISPE-GC/MS法选择性好,快速,净化效果好,灵敏度高,能够快速准确地测定食用油中16种多环芳烃。更多还原

【Abstract】 Objective To establish a method for determination of 16 polycyclic aromatic hydrocarbons( PAHs) in edible oils by gas chromatography-mass spectrometry( GC/MS) combined with molecularly imprinted solid phase extraction( MISPE-GC/MS).Methods Oil samples were diluted with n-hexane,purified by SPE cartridges based on molecularly imprinted polymer.The cartridges were washed by n-hexane to remove impurities,then eluted with dichloromethane.After being concentrated to a volume of 200μL,the analytes were separated by capillary column( 30 m×0.25 mm×0.25 μm) and analyzed by GC/MS with selected ion monitoring( SIM) mode.Isotope internal standard method was adopted for quantification.Results The 16 kinds of PAHs showed good linearity in the range of 2-20 μg/L( r > 0.998).The detection limits ranged from 0.1 to0.6 μg/kg.The recoveries of spiked samples at the level of 2 μg/kg and 10 μg/kg were in the range of 75.5%-125.2%( n = 6),the relative standard deviations( RSD) were all less than 15%.Conclusion The proposed method is selective, fast, and presentsexcellent purification effect as well as high sensitivity,which makes it capable for rapid determination of 16 PAHs in edible oils with satisfactory accuracy.更多还原