Abstract：
BACKGROUND: Mineral oil aromatic hydrocarbon (MOAH) analysis in foods is a major analytical challenge. Quantification is associated with a high uncertainty. The sources of uncertainty are multiple, but the major one is related to data interpretation and integration, which is partially derived from insufficiently efficient sample preparation. Recently, an updated ISO method for the analysis of mineral oil in fats and oils and a standard operating procedure for infant formula analysis have been published. Both methods reported significantly different (up to 1.25) distributions of the internal standards used for quantification (i.e., tri-tert-butyl benzene (TBB) and 2-methyl naphthalene (2-MN)) over the different solvent phases used in the saponification step.
RESULTS: In this work, a microwave-assisted saponification and extraction method was optimized for MOAH analysis to solve the problem related to the MOAH internal standards partition. The paper examines the impact of the solvent mixture used, the concentration of KOH on the partition of TBB and 2-MN, and the effect of the matrix and the washing step to extract the unsaponifiable fraction containing the mineral oils.
CONCLUSIONS: The optimized procedure achieved a TBB/2-MN ratio of 1.05 ± 0.01 tested in five different fats and oils, namely, sunflower, rapeseed, coconut, palm, and extra virgin olive oils. The method can significantly contribute to reducing the uncertainty of the MOAH quantification when saponification is applied.
RESULTS: In this work, a microwave-assisted saponification and extraction method was optimized for MOAH analysis to solve the problem related to the MOAH internal standards partition. The paper examines the impact of the solvent mixture used, the concentration of KOH on the partition of TBB and 2-MN, and the effect of the matrix and the washing step to extract the unsaponifiable fraction containing the mineral oils.
CONCLUSIONS: The optimized procedure achieved a TBB/2-MN ratio of 1.05 ± 0.01 tested in five different fats and oils, namely, sunflower, rapeseed, coconut, palm, and extra virgin olive oils. The method can significantly contribute to reducing the uncertainty of the MOAH quantification when saponification is applied.
摘要：
背景：食品中的矿物油芳烃（MOAH）分析是一项主要的分析挑战。量化与高不确定性相关。不确定性的来源是多重的，但是主要的是数据解释和整合，部分原因是样品制备效率不足。最近,已发布了用于分析脂肪和油中矿物油的最新ISO方法以及用于婴儿配方奶粉分析的标准操作程序。两种方法都报告了用于定量的内标的显着不同（最多1.25）分布（即，三叔丁基苯（TBB）和2-甲基萘（2-MN））在皂化步骤中使用的不同溶剂相中。
结果：在这项工作中，优化了微波辅助皂化提取方法进行MOAH分析，解决了MOAH内标划分的相关问题。本文研究了所用溶剂混合物的影响，KOH在TBB和2-MN分区上的浓度，以及基质和洗涤步骤对提取含矿物油的不皂化物级分的作用。
结论：优化的程序在五种不同的脂肪和油中测试的TBB/2-MN比率为1.05±0.01，即,向日葵,油菜籽,椰子,棕榈,和特级初榨橄榄油。当应用皂化时，该方法可以显着降低MOAH定量的不确定性。
结果：在这项工作中，优化了微波辅助皂化提取方法进行MOAH分析，解决了MOAH内标划分的相关问题。本文研究了所用溶剂混合物的影响，KOH在TBB和2-MN分区上的浓度，以及基质和洗涤步骤对提取含矿物油的不皂化物级分的作用。
结论：优化的程序在五种不同的脂肪和油中测试的TBB/2-MN比率为1.05±0.01，即,向日葵,油菜籽,椰子,棕榈,和特级初榨橄榄油。当应用皂化时，该方法可以显着降低MOAH定量的不确定性。
