气质联用法同时测定烟熏烘烤食品中16种多环芳烃

Simultaneous detection of 16 polycyclic aromatic hydrocarbons in smoked-baked food using gas chromatography-mass spectrometry

目的建立一种快速、高效、准确的测定烟熏烘烤食品中16种欧盟优控多环芳烃(16 EUPAHs)的固相萃取-气质联用法。方法样本经同位素内标稀释后,用环己烷-乙酸乙酯提取,经氢氧化钾-乙醇皂化后,再用正己烷提取,有机相经EUPAHs专用SPE小柱净化后,采用DB-EUPAHs毛细管柱分离,质谱检测器对16种多环芳烃进行检测。结果16种欧盟优控多环芳烃在50~250μg/L范围内有很好的相关性(r>0.9971),最低检出限范围0.03~0.10μg/kg,最低定量限范围为0.10~0.30μg/kg;低浓度组(2μg/kg)回收率范围为84.41%~98.75%,相对标准偏差为3.24%~12.62%(n=6);高浓度组(10μg/kg)回收率范围为87.22%~102.04%,相对标准偏差为4.24%~13.91%(n=6)。结论气质联用法简便、快速、灵敏,可用于烟熏烘烤食品中16种欧盟优控多环芳烃的检测。

Objective To develop a rapid,effective and accurate method for the simultaneous determination of 16 European Union optimal control polycyclic aromatic hydrocarbons(EUPAHs)in smoked-baked food using solid-phase extraction combined with gas chromatography-mass spectrometry(SPE-GC/MS).Methods After dilution by isotopic internal standard,the food sample was extracted with cyclohexane-ethyl acetate,saponified with potassium hydroxide-ethanol and extracted with n-hexane.The organic phase was purified by SPE column dedicated to EUPAHs,and chromatographic separation was performed on a DB-EUPAHs capillary column and detected by GC/MS.Results The 16 EUPAHs showed good linearity in the concentration range of 50-250μg/L(r>0.9971).The limits of detection(LODs)in smoked-baked food of 16 EUPAHs were in the range of 0.03-0.10μg/L and the limits of quantification(LOQs)were between 0.10-0.30μg/L.The recovery rates of the low concentration group(2μg/kg)and the high concentration group(10μg/kg)ranged from 84.41%to 98.75%and 87.22%to 102.04%with the relative standard deviation of 3.24%-12.62%(n=6)and 4.24%-13.91%(n=6).Conclusions SPE-GC/MS is a simple,rapid and sensitive method which can be used for the simultaneous detection of EUPAHs in smoked-baked food.