Validation of a method based on triglycerides for the detection of low percentages of hazelnut oil in olive oil by column liquid chromatography

Abstract

The difference between theoretical and empirical triglyceride content is a powerful tool to detect the presence of any vegetable oil in olive oil. The current drawback of the method is the separation between equivalent carbon number ECN42 compounds, which affects the reliability of the method and, hence, its cutoff limit. The determination of the triglyceride profile by liquid chromatography using propionitrile as the mobile phase has recently been proposed to improve their quantification, together with a mathematical algorithm whose binary response determines the presence or absence of hazelnut oil. Twenty-one laboratories from 9 countries participated in an interlaboratory study to evaluate the performance characteristics of the whole analytical method. Participants analyzed 12 samples in duplicate, split into 3 intercomparison studies. Statistically significant differences due to the experimental conditions were found in some laboratories, which were detected as outliers by use of Cochran's and Grubbs' tests. The relative standard deviations (RSD) for repeatability and reproducibility were determined following the AOAC Guidelines for Collaborative Studies. The analytical properties of the method were determined by means of the sensitivity (0.86), selectivity (0.94), and reliability (72%) for a cutoff limit of 8% (probability 94%).