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

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.