Journal Article

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

Fernández Laespada, María Esther, del Nogal Sánchez, Miguel, Moreno Cordero, Bernardo, Pérez Pavón, José Luis

2009

Overview

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.

• Publisher: Berlin/Heidelberg : Springer-Verlag,Springer-Verlag,Springer
• Subject: Analytical Chemistry / Biochemistry / capillary gas chromatography / Characterization and Evaluation of Materials / Chemistry / Chemistry and Materials Science / Chromatographic methods and physical methods associated with chromatography / detection limit / Detectors / Exact sciences and technology / filtration / Food Science / Gas chromatographic methods / Gas chromatography / Gas Chromatography-Mass Spectrometry - methods / headspace analysis / Heaters / Heptanes - analysis / Hot Temperature / Laboratory Medicine / mass spectrometry / Mathematical analysis / Modular / Monitoring/Environmental Analysis / Olive Oil / Original Paper / Other chromatographic methods / Plant Oils - chemistry / Sensitivity and Specificity / Software / Spectrometric and optical methods / Spectroscopy / Standard deviation / temperature / Volatilization