高效液相色谱法测定烤肉中4种多环芳烃前处理的优化

Optimization of pretreatment of four polycyclic aromatic hydrocarbons in grilled meats by high performance liquid chromatography

采用超声辅助法提取、串联固相萃取柱净化、高效液相色谱法(HPLC)分析烤肉中4种多环芳烃(PAH4,即[艹屈]、苯并[a]蒽、苯并[b]荧蒽、苯并[a]芘)。通过对比固相萃取柱净化效果及回收率、提取剂的提取效果,最终选择ENV柱与SI柱进行串联,正己烷:二氯甲烷(1:1)提取烤肉中PAH4效果更佳,测定结果表明,HPLC法的检出限为0.23~0.32μg/kg,线性范围为5~100μg/L,在3个浓度(2、5μg/L和10μg/L)加标的水平上回收率为77.56%~93.49%,相对标准偏差(RSD,n=6)为0.89%~3.73%。该方法具有前处理简单、快速、线性范围较宽、检测灵敏度高等优点,符合当今食品分析的发展趋势,可广泛应用于烤肉中PAH4的常规监测。

Ultrasound-assisted extraction,series solid phase extraction column purification and high performance liquid chromatography (HPLC) were used to analyze four polycyclic aromatic hydrocarbons (PAH4,chrysene,benzo[a]anthracene,benzo[b]fluoranthene,benzo[a]pyrene) in grilled meats.Compared with the purification effect and recovery rate of the solid phase extraction column and the extraction efficiency of the extractant,the ENV column and the SI column were selected in series,and the hexane: dichloromethane (1:1) was better for extracting PAH4 from the barbecue.The results showed that the detection limit of HPLC method was 0.23~0.32 μg/kg,the linear range was 5~100 μg/L.In 3 different degrees (2,5,10 μg/L),the average recoveries ranged from 77.56%~93.49%,and the relative standard deviations (RSD,n=6) was 0.89%~3.73%.The method has the advantages of simple pretreatment, rapidity,wide linear range and high detection sensitivity,and is in line with the development trend of food analysis today,and can be widely applied to the routine monitoring of PAH4 in grilled meats.