Development of a headspace solid phase microextraction-gas chromatography method for monitoring volatile compounds in extended time-course experiments ... oil [An article from: Analytica Chimica Acta]

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Description:
A novel method for monitoring fibre performance and death, based on a Shewhart control plot, for use in headspace analysis by solid phase microextraction-gas chromatography (SPME-GC) is presented. The method is also demonstrated to be effective in standardising fibre response in extended time-course experiments, where several fibres may be required to complete a lengthy study. Extraction conditions that gave good total recovery and diversity of compounds, from olive oil headspace were found to be: 1g oil sample in 10mL vessel; exposure of DVB-CAR-PDMS, 50/30@mm fibre for 30min at 40^oC; and desorption for 3min at 250^oC. Calibration curves were constructed for 25 compounds commonly reported in olive oil headspace; with coefficients of determination (R^2) ranging from 0.959 to 0.994 and limits of detection (LOD) from 0.01 to 0.59@mg/g. The method was applied to monitor the change in concentration of select C6 volatile compounds, which have implications in sensory quality -E-2-hexenal, hexanal, E-2-hexen-1-ol, hexanol - over a period of 12 months storage.