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目的:建立食用植物油中苯并[α]芘的凝胶色谱-气质联用(GPC-GC/MS)在线测定方法。方法:样品称量后加入苝-d12同位素内标,按约20%(w/v)的比例用GPC流动相溶解后直接在线净化-气质联用法测定。结果:苯乙烯-二乙烯苯共聚的微型凝胶色谱柱与苯并[α]芘之间的大π电子相互作用能有效分离样品中的基体干扰物,方法最低检出浓度(LODs)0.3μg/kg,线性范围1.0μg/kg~100μg/kg,相关系数r=0.9995,回收率90.3%~111%,相对标准偏差(RSD)5.2%~10.7%。结论:本法快速、简便、准确,有机溶剂消耗量少。
Objective: To establish an online method for the determination of benzo [α] pyrene in edible vegetable oil by gel permeation chromatography-gas chromatography-mass spectrometry (GPC-GC / MS). Methods: The sample was weighed and the perylene-d12 isotope internal standard was added. The sample was dissolved in GPC mobile phase at a ratio of about 20% (w / v) and then directly purified by online-GC / MS. Results: The large π-electron interaction between the styrene-divinylbenzene copolymer microgel column and benzo [α] pyrene could effectively separate the matrix interferences from the samples. The minimal detectable concentrations (LODs) of 0.3 μg / kg, the linear range was 1.0μg / kg ~ 100μg / kg, the correlation coefficient was 0.9995, the recovery was 90.3% ~ 111% and the relative standard deviation was 5.2% ~ 10.7%. Conclusion: This method is fast, simple and accurate, with less consumption of organic solvents.