Abstract: Mixed aqueous solutions of 57 volatile compounds were quantitatively analyzed by headspace solid phase microextraction (SPME), in-tube extraction (ITEX), purge trapping (P&T) or static headspace combined with gas chromatography-mass spectrometry (GC-MS). The results showed that 45 compounds were detected by SPME with a polydimethylsiloxane/divinylbenzene (PDMS/DVB)-coated fiber, 41 compounds were detected by ITEX, 31 compounds were detected by Headspace, and 20 compounds were detected by P&T. In general, ITEX more easily detected aldehydes and hydrocarbons (with a quantitation limit of 20 ng/mL for aldehydes and of 10 ng/mL for hydrocarbons), SPME was more sensitive to alcohols and esters (with a quantitation limit of 20 ng/mL for both), and P&T and headspace were more suitable for the quantification of low boiling point compounds. The food matrix had little effect on SPME or ITEX. A combination of SPME and ITEX could effectively improve the completeness and accuracy of the obtained food aroma fingerprint information. The results of this study may provide an experimental basis for food aroma analysis.

Key words: headspace; isotope internal standard; matrix effect; qualitative analysis; quantitative determination