加速溶剂萃取/凝胶渗透色谱净化-气质联用法测定烟熏腊肉中24种多环芳烃

目的 建立烟熏腊肉中24种多环芳烃的气相色谱-质谱联用快速检测方法。方法 腊肉样品与硅藻土充分混合后置于萃取池中加速溶剂萃取,萃取液经过凝胶渗透色谱(GPC)去除油脂,SPE硅胶柱去除极性组分,经DB-EUPAH色谱柱分离后,质谱检测,内标法定量。结果 24种PAHs的线性范围为 1.0～300ng/ml,线性相关系数r为0.9975～0.9999。方法检出限在0.5～5.0μg/kg之间,加标回收率为70.4%～118.5%,相对标准偏差为5.43%～9.74%(n=3)。结论 该方法准确度高,重现性好,适合于烟熏肉中24种PAHs的同时测定。

Determination of 24 Polycyclic Aromatic Hydrocarbons in Smoked meat by ASE extraction-GPC purification combined with gas chromatography-mass spectrometry

Objective To establish a rapid detection method for the detection of 24 PAHs in smoked meat.Methods Sample was mixed with Diatomaceous Earth.The mixtures were put into extract cells to accelerate solvent extraction.The extraction fluid was purified by GPC and SPE column to removed grease and a polar molecule.PAHs were separated by DB-EUPAH chromatography column,analyzed by GC-MS quantified by an internal standard method.Results The result showed that 24 PAHs displayed good linear relationships over the concentration range of 1~300ng/ml,with correlations coefficients more than 0.9975.The limits of detection were 0.5~5.0μg/kg.The average recoveries of 24PAHs at three spiked levels of 10,50,100μg/kg,ranged from 70.4~118.5% with relative deviations of 5.43~9.74%(n=3).Conclusion The method is high accuracy and good reproducibility and is suitable for the simultaneous determination of 24 polycyclic aromatic hydrocarbons(PAHs)in smoked meat.