Optimization of sample clean-up for the determination of small amounts of MOSH and MOAH in edible oils - method DGF C-VI 22 (20).

ABSTRACT

Methods for determining MOSH and MOAH in edible oils showed major problems with interlaboratory comparability of analytical results, especially in the lower concentration range below 10 mg/kg. However, a method with improved sensitivity and reproducibility is urgently needed to obtain a valid data basis for minimization efforts. To cope this problem a new method was created in 2020. The method was established as the standard method DGF C-VI 22 (20) of the German Society for Fat Science e.V. (DGF). For the development of this method different sample epoxidation approaches have been performed, evaluated and improved. Additionally, a saponification, a decision tree for sample preparation, an upstream clean-up column and a system suitability test were introduced. The focus was on reliability and interlaboratory comparability over all edible oil matrices up to a LOQ of 1 mg/kg. The optimized method was validated in terms of trueness and precision in a collaborative trail with 11 laboratories. The achieved recovery rates of 89-105% MOSH and 70-105% MOAH met the JRC requirements. Method and validation results were obtained with HorRat values between 1.3 and 1.8 for MOSH and MOAH.