Ultrasonically assisted solid‐phase extraction and GC analysis of filbertone in hazelnut oil

Abstract

AbstractUltrasound was used to assist solid‐phase extraction (SPE) of filbertone (E‐5‐methylhept‐2‐en‐4‐one) from hazelnut oil. Interferences from TG were reduced for effective separation and detection during chromatographic analysis. The enantiomeric distribution of filbertone was determined. Different sorbent materials, sample volumes, and eluents were tested, and the effect on filbertone recovery by ultrasound during the elution step was evaluated. Experimentation performed on a 2‐mL volume of oil diluted with a 2‐mL volume of n‐hexane, using a silica modified with either a cyano or phenyl group during the extraction, and ultrasound‐assisted elution with a 1‐mL volume of chloroform allowed filbertone recoveries of up to 94.4% (relative SD 6.5%) vs. 11% obtained when ultrasound was not applied. This improvement is most likely due to a mechanism of cavitation. Ultrasonically assisted SPE is proposed as an accesible and simple alternative to multidimensional chromatographic techniques to accomplish the reliable determination of the enantiomeric excess of chiral compounds in complex matrices, such as hazelnut oil, since experimental conditions that can bring about racemization are not required.