Implementing Dynamic Headspace with SPME Sampling of Virgin Olive Oil Volatiles: Optimization, Quality Analytical Study, and Performance Testing

Abstract

Competition and interaction phenomena among volatiles during their adsorption process by solid phase microextraction (SPME) fibers in static headspace sampling procedure (SHS) cast doubt on its ability to quantify virgin olive oil volatiles. SPME fibers being excellent traps, their use was analyzed with a new device allowing the concentration of volatiles in a dynamic headspace sampling procedure (DHS). A central composite experimental design optimized the main variables of the device (4 g sample weight, 40 °C temperature, 150 mL/min flow rate, 50 min adsorption time), while values of the analytical quality control parameters of the method (repeatability, limits of detection and quantification, working range, sensitivity, and resolution) were compared with those ones from static headspace. DHS shows better precision results for aldehydes and alcohols than SHS and allowed analyzing higher concentrations with no problem of saturation. In 19 of 28 compounds analyzed in 50 samples the chromatographic areas were higher when running DHS. The concentration values of volatile compounds in these samples after applying SHS and DHS are discussed together with the ability of the new method for distinguishing virgin olive oil by their categories (extra virgin, virgin, and lampante) by the volatiles quantified in commercial oils.