Facile separation and enrichment of polychlorinated biphenyls (PCBs) in foods has been a constantly pursuing goal in food analytical chemistry. Here, a reusable ionic liquid functionalized magnetic graphene oxide nanocomposite (3D-IL@mGO), synthesized based on our previous study, was used as adsorbent for the preconcentration of PCBs in the magnetic dispersive solid phase extraction (Mag-dSPE) procedure. Comparing the proposed 3D-IL@mGO Mag-dSPE procedure with carboxylated multiwalled carbon nanotubes d-SPE method, the 3D-IL@mGO nanocomposite could be reused at least 16 times for the extraction of 11 PCBs from seafood samples without significant sacrifice of the extraction efficiency, which is more economical. Under the optimal conditions, a simple analytical method based on Mag-dSPE and gas chromatography-triple quadrupole mass spectrometry (GC–MS/MS) has been developed for the fast determination of 11 polychlorinated biphenyls (PCBs) in seafood. The LODs for 11 PCBs were in the range of 0.012 μg·kg⁻¹–0.054 μg·kg⁻¹. The recoveries were ranged from 80.0% to 112% with associated intra-day and inter-day relative standard deviations (RSDs) in the range of 2.7%-6.2% and 3.6%-7.3%, respectively. Furthermore, the proposed method was applied for the analysis of 11 PCBs in 240 seafood samples. The results showed that PCB 101, PCB 153 and PCB 204 were found in 18 seafood samples with concentrations ranged from 0.862 μg·kg⁻¹ to 12.1 μg·kg⁻¹. It is, therefore, concluded that the Mag-dSPE procedure combined with GC–MS/MS demonstrated the applicability for food-safety risk monitoring of PCBs in seafood samples.

轻松分离和富集食品中的多氯联苯 (PCB) 一直是食品分析化学领域不断追求的目标。在这里，基于我们之前的研究合成的可重复使用的离子液体功能化磁性氧化石墨烯纳米复合材料（3D-IL@mGO）被用作吸附剂，用于在磁分散固相萃取（Mag-dSPE）程序中预浓缩多氯联苯。将提议的 3D-IL@mGO Mag-dSPE 程序与羧化多壁碳纳米管 d-SPE 方法进行比较，3D-IL@mGO 纳米复合材料可以重复使用至少 16 次，从海鲜样品中提取 11 种 PCB，而不会显着牺牲提取效率更高，更经济。在最优条件下，开发了一种基于 Mag-dSPE 和气相色谱-三重四极杆质谱 (GC-MS/MS) 的简单分析方法，用于快速测定海鲜中的 11 种多氯联苯 (PCB)。11 种 PCB 的 LOD 范围为 0.012 μg·kg^-1 –0.054 μg·kg ^-1。回收率范围为 80.0% 至 112%，相关的日内和日间相对标准偏差 (RSD) 分别在 2.7%-6.2% 和 3.6%-7.3% 的范围内。此外，该方法还用于分析 240 份海鲜样品中的 11 种多氯联苯。结果表明，PCB 101、PCB 153 和PCB 204 在18 个海鲜样品中检出，浓度范围为0.862 μg·kg ^-1至12.1 μg·kg ^-1。因此得出的结论是，Mag-dSPE 程序与 GC-MS/MS 相结合证明了海鲜样品中 PCB 食品安全风险监测的适用性。