The extraction of aroma volatile compounds was performed through the in-tube extraction technique (ITEX) and the analysis was carried out on a GCMS QP-2010 gas chromatograph-mass spectrometer instrument (Shimadzu Scientific Instruments, Kyoto, Japan) as described in our previous works [77 (link),78 (link)]. Briefly, 3 g of each sample was introduced into a headspace vial of 20 mL, incubated for 20 min at a temperature of 60 °C, and the volatile compounds in the gas phase were absorbed through a fiber syringe (ITEX-2TRAPTXTA, Tenax TA 80/100 mesh) and directly desorbed into the GC-MS injector.
A Zebron ZB-5MS (Phenomenex) capillary column was used for the separation of the volatile compounds with helium as the carrier gas, a split ratio of 1:5, and a flow rate of 1 mL/min. The chromatographic column program was as follows: 35 °C (for 5 min) rising to 155 °C with 7 °C/min and then heated to 260 °C with 10 °C/min and held for 5 min. NIST27 and NIST147 mass spectra libraries were used for identifying the spectra of the reference compounds and checked by comparison with retention indices drawn fromwww.pherobase.com or www.flavornet.org [79 ,80 ]. The peaks that were identified at least in two of the three total ion chromatograms (TIC) were considered in calculating the total area of peaks (100%) and the relative areas of the volatile compounds [44 (link)].
A Zebron ZB-5MS (Phenomenex) capillary column was used for the separation of the volatile compounds with helium as the carrier gas, a split ratio of 1:5, and a flow rate of 1 mL/min. The chromatographic column program was as follows: 35 °C (for 5 min) rising to 155 °C with 7 °C/min and then heated to 260 °C with 10 °C/min and held for 5 min. NIST27 and NIST147 mass spectra libraries were used for identifying the spectra of the reference compounds and checked by comparison with retention indices drawn from
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