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Determination of filbertone in spiked olive oil samples using headspace-programmed temperature vaporization-gas chromatography-mass spectrometry

Pérez Pavón, José Luis, del Nogal Sánchez, Miguel, Fernández Laespada, María Esther, Moreno Cordero, Bernardo
Analytical and bioanalytical chemistry 2009 v.394 no.5 pp. 1463-1470
capillary gas chromatography, detection limit, filtration, headspace analysis, mass spectrometry, olive oil, temperature
A sensitive method for the fast analysis of filbertone in spiked olive oil samples is presented. The applicability of a headspace (HS) autosampler in combination with a gas chromatograph (GC) equipped with a programmable temperature vaporizer (PTV) and a mass spectrometric (MS) detector is explored. A modular accelerated column heater (MACHTM) was used to control the temperature of the capillary gas chromatography column. This module can be heated and cooled very rapidly, shortening total analysis cycle times to a considerable extent. The proposed method does not require any previous analyte extraction, filtration and preconcentration step, as in most methods described to date. Sample preparation is reduced to placing the olive oil sample in the vial. This reduces the analysis time and the experimental errors associated with this step of the analytical process. By using headspace generation, the volatiles of the sample are analysed without interference by the non-volatile matrix, and by using injection in solvent-vent mode at the PTV inlet, most of the compounds that are more volatile than filbertone are purged and the matrix effect is minimised. Use of a liner packed with Tenax-TA® allowed the compound of interest to be retained during the venting process. The limits of detection and quantification were as low as 0.27 and 0.83 μg/L, respectively, and precision (measured as the relative standard deviation) was 5.7%. The method was applied to the determination of filbertone in spiked olive oil samples and the results revealed the good accuracy obtained with the method.