加速溶剂萃取-凝胶渗透色谱-气相色谱-串联质谱法测定中华绒鳌蟹中16种多环芳烃

Determination of 16 kinds of polycyclic aromatic hydrocarbons in Eriocheir sinensis by accelerated solvent extraction-gel permeation chromatography-gas chromatography-tandem mass spectrometry

目的建立气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)测定中华绒鳌蟹中16种多环芳烃(polycyclic aromatic hydrocarbons,PAHs)的分析方法。方法中华绒螯蟹样品与硅藻土研磨混匀后经加速溶剂萃取(accelerated solvent extraction,ASE)仪提取,使用凝胶渗透色谱法(gel permeation chromatography,GPC)净化,全自动浓缩仪在线浓缩后,在多级离子反应监测(multistage ion reaction monitoring,MRM)模式下分析,采用同位素内标法进行定量。结果16种PAHs在1~100 ng/mL范围内线性关系良好,相关系数(r)≥0.995。定量限在0.3~0.5μg/kg之间,在1.0、2.0、10.0μg/kg 3个加标水平下,16种PAHs的平均加标回收率为80.3%~05.4%,相对标准偏差(relative standard deviation,RSD)≤10.3%。结论该方法自动化程度高、准确、稳定、可靠,可用于测定中华绒螯蟹中16种PAHs的残留量。

Objective To establish a method for the determination of 16 polycyclic aromatic hydrocarbons(PAHs)in Eriocheir sinensis using gas chromatography-tandem mass spectrometry(GC-MS/MS).Methods The samples of Eriocheir sinensis were mixed and ground with diatomite and extracted by accelerated solvent extraction(ASE),purified by gel permeation chromatography,and concentrated online by automatic thickener.The target compounds were quantified using an isotopic internal standard in the mode of multistage ion reaction monitoring(MRM).Results The 16 kinds of polycyclic aromatic hydrocarbons showed good linear relationships in the range of 1-100 ng/mL.The correlation coefficients were all equal or greater than 0.995.The limits of quantitation(LOQs)were 0.3-0.5μg/kg and the average recoveries of 16 kinds of polycyclic aromatic hydrocarbons were 80.3%-105.4%at the 3 kinds of spike levels of 1.0,2.0,10.0μg/kg.The relative standard deviations(RSDs)were equal or less than 10.3%.Conclusion This method is highly automatic,accurate,stable and reliable,and can be used for monitoring 16 kinds of PAHs in Eriocheir sinensis.