This study compares three headspace-based extraction techniques—Regular solid-phase microextraction (HS- SPME), vacuum-assisted SPME (Vac-HS-SPME), and probe-type sorptive extraction (HiSorb)—for the analysis of volatile organic compounds (VOCs) in virgin olive oil (VOO). Using a combined untargeted–targeted GC × GC–MS approach, 34 VOCs were selected. Vac-HS-SPME enhanced recovery of semi-volatile compounds linked to oxidative and microbiological defects, underrepresented by HS-SPME and HiSorb. Conversely, HS- SPME and HiSorb preferentially extracted low-molecular-weight lipoxygenase (LOX)-derived volatiles associated with green and fruity notes, with HiSorb showing broader coverage and stronger alcohol and aldehyde responses. ANOVA and Tukey's post hoc test (p < 0.05) indicated significant differences among techniques for 24 analytes. These findings provide method-oriented insights into VOC-based workflows for olive oil profiling and suggest the potential applicability of targeted headspace applications in quality control, classification, and sensory characterization of VOO.
This study compares three headspace-based extraction techniques—Regular solid-phase microextraction (HS-SPME), vacuum-assisted SPME (Vac-HS-SPME), and probe-type sorptive extraction (HiSorb)—for the analysis of volatile organic compounds (VOCs) in virgin olive oil (VOO). Using a combined untargeted–targeted GC × GC–MS approach, 34 VOCs were selected. Vac-HS-SPME enhanced recovery of semi-volatile compounds linked to oxidative and microbiological defects, underrepresented by HS-SPME and HiSorb. Conversely, HS-SPME and HiSorb preferentially extracted low-molecular-weight lipoxygenase (LOX)-derived volatiles associated with green and fruity notes, with HiSorb showing broader coverage and stronger alcohol and aldehyde responses. ANOVA and Tukey's post hoc test (p < 0.05) indicated significant differences among techniques for 24 analytes. These findings provide method-oriented insights into VOC-based workflows for olive oil profiling and suggest the potential applicability of targeted headspace applications in quality control, classification, and sensory characterization of VOO.
Comparison of headspace pre-concentration techniques for volatile profiling of virgin olive oil by comprehensive two-dimensional chromatography
Spadafora, Natasha Damiana;
2026
Abstract
This study compares three headspace-based extraction techniques—Regular solid-phase microextraction (HS-SPME), vacuum-assisted SPME (Vac-HS-SPME), and probe-type sorptive extraction (HiSorb)—for the analysis of volatile organic compounds (VOCs) in virgin olive oil (VOO). Using a combined untargeted–targeted GC × GC–MS approach, 34 VOCs were selected. Vac-HS-SPME enhanced recovery of semi-volatile compounds linked to oxidative and microbiological defects, underrepresented by HS-SPME and HiSorb. Conversely, HS-SPME and HiSorb preferentially extracted low-molecular-weight lipoxygenase (LOX)-derived volatiles associated with green and fruity notes, with HiSorb showing broader coverage and stronger alcohol and aldehyde responses. ANOVA and Tukey's post hoc test (p < 0.05) indicated significant differences among techniques for 24 analytes. These findings provide method-oriented insights into VOC-based workflows for olive oil profiling and suggest the potential applicability of targeted headspace applications in quality control, classification, and sensory characterization of VOO.I documenti in SFERA sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
