Nutrition and Bromatology Group, Analytical and Food Chemistry Department, Faculty of Food Science and Technology, University of Vigo, Ourense Campus, 32004 Ourense, Spain.
Food Chem. 2013 Aug 15;139(1-4):1036-43. doi: 10.1016/j.foodchem.2013.02.012. Epub 2013 Feb 16.
Fish oil has been identified as one of the most important contributors to the level of Persistent Organic Pollutants (POPs) in feed products. The determination of polycyclic aromatic hydrocarbons (PAHs) in fish oils is complicated due to the fat matrix, which affects both extraction efficiency and analytical quality. This article reviews and addresses two of the most relevant analytical methods for determining 11 mutagenic and carcinogenic PAHs, as well as two EPA indicator PAHs in fish oils. We discuss and critically evaluate two different extraction procedures, such as ultrasound-assisted solvent extraction (USAE) and ultrasound-assisted emulsification-microextraction (USAEME). Clean-up of extracts was performed by solid-phase extraction using C18 and glass columns containing silica gel and florisil for USAE or only C18 for USAEME. Detection of the selected PAHs was carried out by high-performance liquid chromatography coupled with fluorescence detection for determination. Optimization of the variables affecting extraction by the selected extraction techniques was conducted and recoveries ranged from 70% to 100% by USAE and from 70% to 108% by USAEME with estimated quantification limits between 0.020 and 2.6 μg/kg were achieved. Moreover, the applicability of the selected methods was evaluated by the analysis of real samples. To our knowledge, this is the first time that USAEME has been applied to the determination of PAHs in food matrices, such as oil fish samples. The methods proposed were applied to the determination of the target PAHs in fish samples from different countries, and it was found that the low PAH contamination of the selected fish oils could mainly occur by atmospheric sources.
鱼油已被确定为饲料产品中持久性有机污染物(POPs)水平的最重要贡献者之一。由于脂肪基质的影响,鱼油中多环芳烃(PAHs)的测定较为复杂,这会影响提取效率和分析质量。本文综述并讨论了两种最相关的分析方法,用于测定鱼油中的 11 种致突变和致癌多环芳烃以及两种 EPA 指示性多环芳烃。我们讨论并批判性地评估了两种不同的提取程序,例如超声辅助溶剂提取(USAE)和超声辅助乳化-微萃取(USAEME)。通过使用 C18 和玻璃柱中的硅胶和 Florisil 进行固相萃取(SPE)对提取物进行净化,C18 用于 USAEME 或仅用于 USAE。通过高效液相色谱法(HPLC)与荧光检测联用对所选 PAHs 进行检测。通过所选提取技术对影响提取的变量进行了优化,回收率通过 USAE 为 70%至 100%,通过 USAEME 为 70%至 108%,并实现了 0.020 至 2.6 μg/kg 之间的估计定量限。此外,通过对实际样品的分析评估了所选方法的适用性。据我们所知,这是首次将 USAEME 应用于鱼油样品等食品基质中 PAHs 的测定。所提出的方法已应用于不同国家的鱼样中目标 PAHs 的测定,发现所选鱼油中低水平的 PAH 污染主要可能来自大气源。