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Novel fast analytical method for indirect determination of MCPD fatty acid esters in edible oils and fats based on simultaneous extraction and derivatization

机译:基于同时萃取和衍生化的间接测定食用油脂中MCPD脂肪酸酯的快速分析新方法

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摘要

A novel method for indirect determination of MCPD esters levels in lipid samples has been developed. The method is based on combination of extraction and derivatization in the same sample preparation step. It is achieved by the application of diethyl ether as extraction solvent for isolation of analytes released from esterified forms from the water phase and as dilution solvent for solid PBA – the derivatization agent. It is a noteworthy improvement of recommended indirect approaches available in the literature because such steps as sample clean-up, multiple liquid–liquid extractions, and preconcentration are excluded in the proposed solution. In this way, the developed procedure is shortened and simplified. Such an approach also minimizes the utilization of organic solvents; therefore, it is in accordance with the principles of “green analytical chemistry.” In spite of the fact that the step of sample clean-up is omitted, no deterioration in GC-MS system performance was observed. Equivalence testing of the developed procedure and AOCS cd 29b-13 official method (SGS) has been conducted. It was concluded that results obtained by both methods do not significantly differ statistically. The procedure has been applied to determination of MCPD esters concentrations in lipid fractions isolated by accelerated solvent extraction technique from such foodstuffs as bakery products, salty deep-fried snacks, and instant products. In all investigated samples, the level of bound MCPD was elevated. Additionally, for both procedures, the environmental impact (with the use of analytical Eco-scale) and uncertainty budget have been assessed and compared.
机译:已经开发了一种间接测定脂质样品中MCPD酯水平的新方法。该方法基于同一样品制备步骤中提取和衍生化的组合。它通过使用乙醚作为萃取溶剂来分离从水相中酯化形式释放的分析物,以及用作固体PBA(衍生试剂)的稀释溶剂而实现。这是文献中推荐的间接方法的显着改进,因为建议的解决方案中不包括样品净化,多次液-液萃取和预浓缩等步骤。这样,可以缩短和简化开发的过程。这种方法还可以最大程度地减少有机溶剂的利用。因此,它符合“绿色分析化学”的原则。尽管省略了样品清理步骤,但未观察到GC-MS系统性能下降。已对开发的程序和AOCS cd 29b-13官方方法(SGS)进行了等效测试。结论是,两种方法获得的结果在统计学上均无显着差异。该方法已用于测定通过加速溶剂萃取技术从诸如烘焙食品,咸炸小吃和速溶食品等食品中分离的脂质级分中MCPD酯的浓度。在所有研究的样品中,结合的MCPD水平升高。此外,对于这两个程序,已经评估并比较了环境影响(使用分析型生态规模)和不确定性预算。

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