Influence of different extraction parameters on a solid-phase dynamic extraction for the gas chromatographic determination of d-limonene degradation products by using a fractional factorial design

Through the application of a solid-phase dynamic extraction (SPDE) method for the determination of volatile substances, different parameters may influence the extraction and desorption process and are, therefore, vital for the determination of the extracted substances via gas chromatography (GC). In this study, the influence of extraction und desorption parameters of an SPDE-GC method for the determination of the d-limonene degradation products, namely, alpha-terpineol, (-)-carveol, and (S)-carvone, in an aqueous model system was evaluated using a factorial fractional design. The aim was to reduce the number of factors that should be considered for the optimization of an SPDE procedure for different applications. It could be shown that the extraction efficiency of alpha-terpineol, (-)-carveol, and (S)-carvone is significantly influenced by the extraction parameters incubation temperature, number of extraction strokes, and amount of added NaCl. All 3 parameters have a positive effect on the extraction and determination of the examined d-limonene degradation products. Due to the identification of significant factors on the basis of an experimental design, the results of this study can be very useful for further development of SPDE methods for different applications.