College of Public Health and Management, Wenzhou Medical University, Wenzhou, 325035, Zhejiang, China.
National and Local Joint Engineering Laboratory of Municipal Sewage Resource Utilization Technology, School of Environmental Science and Engineering, Suzhou University of Science and Technology, Suzhou, 215009, Jiangsu, China.
Anal Bioanal Chem. 2021 Mar;413(7):1983-1997. doi: 10.1007/s00216-021-03167-0. Epub 2021 Jan 23.
Herein, we developed a novel effervescence-assisted dual microextraction method, abbreviated as EM-LPSH, using lighter-than-water phosphonium-based ionic liquids (LPILs) and switchable hydrophilic/hydrophobic fatty acids (SHFAs). The EM-LPSH method was utilized for quick enrichment/extraction of polycyclic aromatic hydrocarbons (PAHs) in edible oils. Owing to lower density than water, LPILs used as the first extractant were floated on the upper layer of the aqueous phase, leading to a convenient separation/collection compared with traditional heavier-than-water imidazolium-based ionic liquids. Interestingly, SHFAs play triple functions: a dispersive solvent in the microextraction process, an acidic source in effervescent reaction, and the second extractant in dual microextraction, due to switchability from hydrophilicity to hydrophobicity. Consequently, the integration of LPILs with SHFAs greatly enhanced the extraction efficiency for PAHs owing to the quick dual microextraction process. Some important variables were rigorously optimized using a one-factor-at-a-time approach. Under optimized conditions, the EM-LPSH/HPLC-FLD method provided a wide linear range (0.07~0.63-200 μg kg), satisfactory recovery (80.12-103.27%), and low limit of detection (0.02-0.19 μg kg), as well as high intra-day and inter-day precision (0.03-6.55) for six PAHs in edible oils. By using certified reference material in olive oil samples (GBW10162), the recoveries ranged from 97.40 to 98.39%, demonstrating high accuracy and precision. According to the detected levels of PAHs in six unheated and heated oils, their edible safety was evaluated in detail. In short, the newly developed method is simple, convenient, and highly efficient, thereby showing great prospects for application in conventional monitoring of trace-level PAHs in edible oils.
在此,我们开发了一种新颖的鼓泡辅助双微萃取方法,简称 EM-LPSH,使用轻于水的磷鎓基离子液体(LPILs)和可切换亲/疏水脂肪酸(SHFAs)。该 EM-LPSH 方法用于快速富集/提取食用油中的多环芳烃(PAHs)。由于密度小于水,用作第一萃取剂的 LPILs 浮在水相上层,与传统重于水的咪唑鎓基离子液体相比,分离/收集更加方便。有趣的是,SHFAs 具有三重功能:在微萃取过程中作为分散溶剂,在鼓泡反应中作为酸性源,并且在双微萃取中作为第二萃取剂,由于其可从亲水性切换到疏水性。因此,由于快速的双微萃取过程,LPILs 与 SHFAs 的结合极大地提高了 PAHs 的萃取效率。使用单因素法严格优化了一些重要变量。在优化条件下,EM-LPSH/HPLC-FLD 方法为 6 种食用油中的 PAHs 提供了宽线性范围(0.07~0.63-200μgkg)、满意的回收率(80.12-103.27%)和低检测限(0.02-0.19μgkg),以及高日内和日间精密度(0.03-6.55)。通过使用橄榄油样品中的认证参考物质(GBW10162),回收率范围为 97.40-98.39%,表明具有高精度和高准确度。根据 6 种未加热和加热油中 PAHs 的检出水平,详细评估了它们的食用安全性。简而言之,新开发的方法简单、方便、高效,因此在常规监测食用油中痕量 PAHs 方面具有广阔的应用前景。