Fatty acid ethyl esters (FAEE) in virgin olive oil: A shorter and full validated approach as an alternative to the EU Official Method

Abstract

In this work a SPE/GC-FID method, incorporating the use of a 1-g silica cartridge, for the determination of FAEE in olive oils is presented. The procedure has been fully validated, initially 'in-house' and subsequently by an international validation study involving sixteen laboratories from Europe, the United States of America, and China. Key performance parameters of the method are: (1) Linearity in the 10-134 mg/kg range (R² > 0.999), (2) LOD and LOQ < 0.5 mg/kg, (3) RSD_r < 10%, (4) RSD_R < 20% (for 4 out of 5 test materials). In addition, the method has been demonstrated to provide equivalent results to the Official Method (Commission Regulation 2568/91) while providing advantages in terms of reductions in time and solvents and ease of automation. In fact, the proposed protocol requires 30 mL solvents and takes 1.5 h per determination instead of the 350 mL and 6 h needed in the UE Official Method.

Keywords: Ethyl linoleate (PubChem CID: 5282184); Ethyl oleate (PubChem CID: 5363269); Ethyl palmitate (PubChem CID: 12366); Ethyl stearate (PubChem CID: 8122); Fatty acid ethyl esters (FAEE); Fraud detection; Method validation; Methyl heptadecanoate (PubChem CID: 15609); OLEUM; Olive oil; Soft deodorization.