Quantitative Analysis of aliphatic aldehydes by headspace SPME sampling and ion-trap GC-MS

Summary A fast and simple headspace SPME sampling method has been developed for quantification of volatile aliphatic aldehydes in sunflower oil. Analysis has been performed by gas chromatography, on a 30m×0.25 mm i.d. ×0.25 μm CP-Wax 52CB column, with mass spectrometric detection. Carryover from the SPME fiber could be eliminated by heating the fiber in the injection port between runs. Response factors of all the compounds were linear for concentrations up to 100 ng μL⁻¹. The slopes of the calibration curves decrease with the amount of saturation of the aldehydes. The average responses for unsaturated aldehydes were twice as high as those for the saturated variety. Responses for dienes were approximately one order of magnitude higher than for saturated aldehydes. Depletion of the analyte was examined by repeated extraction from the same vial. SPME was optimized—after 30 min extraction most components were found to have reached equilibration. The detection limit for the compounds studied varied between 0.1 and 1 ng μL⁻¹. Distribution constants were determined for ten different aldehydes and Henry's constants were calculated for unsaturated aldehydes. There was a definite relationship between the response factors and the amount of saturation of the aldehydes. Presented at: Balaton Symposium on High-Performance Separation Methods, Siófok, Hungary, September 3–5, 1997