2种前处理技术/气相色谱-质谱技术测定食用植物油中16种多环芳烃残留量及其对比研究

Comparative study on determination of polycyclic aromatic hydrocarbons in edible vegetable oil by 2 kinds of pretreatment methods/gas chromatography-mass spectrometry

目的比较2种前处理技术/气相色谱-质谱技术测定食用植物油中16种多环芳烃残留量。方法本研究利用QuEChERS(quick,easy,cheap,effective,ruggedandsafe)和凝胶渗透色谱(gelpermeation chromatography, GPC)2种前处理技术对样品进行处理,并采用16种多环芳烃全指标同位素内标法定量。比较使用QuEChERS和GPC 2种不同前处理方法的净化效果和方法学参数。结果 16种多环芳烃在10～200 ng/mL范围内线性关系良好,相关系数均大于0.995,定量限为0.3～0.8μg/kg。使用QuEChERS前处理方法的平均回收率和相对标准偏差(relative standard deviation, RSD)分别为88.9%～112.3%和3.6%～12.9%,使用GPC方法的平均回收率和RSD分别为86.2%～107.7%和3.0%～7.3%。对实验室内食用植物油样品进行测定, 2种方法检测结果基本一致。结论 2种前处理方法的精确度和稳定性均较好,均可用于食用植物油中16种多环芳烃残留量的测定。

Objective To compare the determination of 16 kinds of polycyclic aromatic hydrocarbons(PAHs) in edible vegetable oil by 2 kinds of pretreatment methods/gas chromatography-mass spectrometry(GC-MS). MethodsThe samples were pretreated by 2 kinds of methods including QuEChERS(quick, easy, cheap, effective, rugged and safe) and gel permeation chromatography(GPC) methods. The 16 PAHs were quantified by isotopic internal standard method. The purification effect and methodological parameters of 2 different pretreatment methods of QuEChERS and GPC were compared. Results Sixteen PAHs had good linear relationships in the range of 10-200 ng/mL with the correlation coefficients were greater than 0.995. The limits of quantitation(LOQs) were in the range of 0.3-0.8 μg/kg. The average recoveries were 88.9%-112.3% with the relative standard deviations(RSDs) of 3.6%-12.9% when QuEChERS was used as pretreatment method. The average recoveries were 86.2%-107.7% with the RSDs of 3.0%-7.3% by using GPC. The determination results of edible vegetable oil samples using 2 different pretreatments in the laboratory were basically the same. Conclusion The 2 kinds of different pretreatment methods are accurate and stable, which can be used for the determination of 16 kinds of PAHs residues in edible vegetable oil.