Determination of 3-Monochloropropane-1,2-Diol Esters in Edible OilaEuro center dot Method Validation and Estimation of Measurement Uncertainty

摘要

A gas chromatography mass spectrometry (GC-MS) method was developed and validated for the determination of the sum of 3-monochloropropane-1,2-diol (3-MCPD) esters in edible oils. Meanwhile, the measurement uncertainty was estimated. Testing sample preparation was optimized, and the optimal condition was attained. Good linearity was observed with the GC-MS method for the concentration range of 0.05-5.0 mg/kg (R (2) = 0.9994). It was proved to be an accurate and precise method for the determination of 3-MCPD esters according to the validation results. The recovery range was 89.0-104.6 %, and the limits of detection (LOD) and the limits of quantification (LOQ) were 25 and 50 mu g/kg, respectively. Satisfactory reproducibility was achieved with lower than 15 %. Repeatability was determined and expressed as relative standard deviation (RSD), with the value range of 3.9-12.0 %.The contents of 3-MCPD esters were determined in 12 kinds of oils using this method. Measurement uncertainties were calculated by applying bottom-up approach. The main dominant sources were identified and quantified, which were standard solutions preparation, recovery, and calibration curve. It reminds that the predominant uncertainty sources should be paid much more attention during preparing the testing samples in the future.