基于多壁碳纳米管作为吸附剂的分散固相萃取/ GC-MS对食用植物油中16种多环芳烃的 快速测定Rapid determination of 16 polycyclic aromatic hydrocarbons in edible vegetable oil by d-SPE/GC-MS with multi-walled carbon nanotubes as adsorbents

为了快速检测食用植物油中的16种多环芳烃（PAHs)，以氨基化多壁碳纳米管（NH2-MWCNTs）作为样品前处理的吸附剂，采用分散固相萃取（d-SPE）/气相色谱-质谱联用（GC-MS）同时测定食用植物油中的16种PAHs。通过单因素实验对样品前处理条件（吸附剂用量、吸附时间、洗脱剂类型及用量、洗脱时间）进行了优化，对所建立的方法进行了方法学考察，并与已有检测方法进行了对比分析，同时采用所建立的方法对实际样品进行了测定。结果表明：样品前处理最优条件为吸附剂用量15 mg(样品食用植物油质量1.0 g)、吸附时间1 min、洗脱剂甲苯、洗脱剂用量500 μL、洗脱时间5 min；16种PAHs在1～200 μg/kg范围内线性关系良好，方法的检出限在0.05～043 μg/kg之间，定量限在0.17～1.42 μg/kg，加标回收率和相对标准偏差分别为70.67%～10183%和1.34%～9.32%；与已有前处理方法相比，d-SPE高效、简便，且最大程度地减少了有机溶剂的消耗；6种市售食用植物油中苯并\[a\]芘含量均小于2 μg/kg。综上，所建立的方法适用于食用植物油中16种PAHs的测定。To rapidly detect 16 polycyclic aromatic hydrocarbons (PAHs) in edible vegetable oil, the aminated multi-walled carbon nanotubes (NH2-MWCNTs) were used as adsorbents for sample pretreatment, and the dispersion solid phase extraction (d-SPE) with GC-MS method was developed for the simultaneous determination of 16 PAHs in edible vegetable oil samples. The sample pretreatment conditions (the adsorbent dosage, adsorption time, the type and amount of eluent, elution time) were optimized by single factor experiments, and the methodology of the established detection method was investigated and compared with existing methods. Meanwhile, actual samples were detected using the established method. The results showed that the optimal conditions for sample pretreatment were as follows: adsorbent dosage 15 mg (for 1.0 g edible vegetable oil sample), adsorption time 1 min, toluene as the eluent, eluent dosage 500 μL, elution time 5 min. The 16 PAHs showed good linear relationship in the range of 1-200 μg/kg, and the detection limits of the method ranged from 0.05 μg/kg to 0.43 μg/kg, with quantitative limits between 0.17 μg/kg and 1.42 μg/kg. The spiked recovery rate and relative standard deviation were 70.67%-101.83% and 1.34%-9.32%, respectively. Compared to existing pretreament methods, d-SPE is efficient, simple and minimizes the consumption of organic solvents. The content of benzo \[a\] pyrene in 6 commercial edible vegetable oils was less than 2 μg/kg. In summary, the established method is suitable for the determination of 16 PAHs in edible vegetable oil.