Finnigan trace gc ultra

Volatile components of EOs and hexane extracts were analyzed using Finnigan Trace GC Ultra (Thermo Fisher Scientific, Waltham, MA, USA) equipped with a Phenomenex Zebron ZC-5 MS (Phenomenex, Torrance, CA, USA) capillary column (5% phenyl, 95% methyl poly siloxane, 30 m × 0.25 mm × 0.25 µm film thickness) and a DSQ quadrupole mass detector (Thermo Fisher Scientific, Waltham, MA, USA). The volatile components were further detected using MS with an electron impact ionization positive mode at 70 eV. The temperature of the electron ionization ion source and injection port was maintained at 230 and 240 °C, respectively, whereas the column’s initial temperature was kept at 60 °C for 3 min and then further increased 3 °C/min until it reached 240 °C. Helium (>99% purity) was used as a carrier gas with a flow velocity of 1 mL/s. A sample dissolved in methanol (1 μL, concentration = 1 mg/mL) was injected with a Finnigan Autoinjector AI3000 (Thermo Fisher Scientific, Waltham, MA, USA) with split ratio of 1:10. The detection of the components was performed by comparing the MS spectra sample with the NIST05 and Adams EO library. The percentage abundance of each identified component was determined based on the percentage area normalization method.

ET content was determined according to López-Gálvez et al. (2015) (link). A gas chromatograph with flame ionization detector was used (GC-FID) (Finnigan Trace GC Ultra, Thermo Fisher Scientific, Waltham, United States) equipped with the columns15 m/0.53 mm/RT-MSieve 5A (Restek, Bellefonte, United States), 30 m/RTU-Piot (Restek), and 25 m/0.53 mm/CP-PoraBOND Q Fused Silica (Varian, PaloAlto, United States). After calibration of the equipment, samples (∼1 mL) of headspace from weighed chopped material were injected into the column using a gas syringe. The GC oven was set at a constant temperature of 35°C, the carrier gas was helium and the FID used pressurized hydrogen and air. The software Thermo Finnigan Chrom Card32-bit was used to interpret the results.

All reaction products (FFA, partial acylglycerols and TAG) were separated by silica gel thin-layer chromatography (TLC). The TAG band was recovered, methylated and analysed by gas chromatography (GC), as fatty acid methyl esters (FAME), according to the methodology described by [36 (link)]. A gas chromatograph Finnigan TRACE GC Ultra (Thermo Electron Corporation) with a capillary column (60 m × 0.25 mm ID × 0.25 µm film) Thermo TR-FAME, and an AS 3000 autosampler from Thermo Electron Corporation were used for FAME analysis. The flame ionization detector (FID) was set at 280 °C and supplied with air and hydrogen at 350 and 35 mL min⁻¹, respectively, The injector (in splitless mode) was set at 250 °C. The temperature program of the chromatographic column was the following: 100 °C for 1 min, increase to 160 °C at 10 °C min⁻¹, held for 10 min, increase to 235 °C at 4 °C min⁻¹ and kept for 10 min. The carrier gas Helium was supplied at a flow rate of 1.2 mL min⁻¹. Fatty acid methyl ester mixes (PUFA No1 and PUFA No 3, from Supelco) were used as external standard and methyl myristate (C14:0) as internal standard.
The incorporation degree (ID) of C8:0 or C10:0 in TAG of argan oil, was calculated as follows, Equation (1) [20 (link)]: $$ID (\%)=\left(\frac{\mathrm{MFA}}{\mathrm{MT}}\right)\times 100$$
where MFA represents the C8:0 or C10:0 moles in the TAG and MT is the total amount of fatty acids (moles) in the TAG.

The system used for identification of compounds was a Finnigan Trace GC Ultra (Thermo Electron Corporation/Thermo Scientific) coupled to a Thermo DSQ Single Quadrupol MS (Thermo Electron Corporation/Thermo Scientific), equipped with a Gerstel MPS 2 auto sampler. The software for mass spectral recording and data analysis was the Xcalibur Data System (Version1.4, Thermo Electron Corporation/Thermo Scientific). The analytical capillary used was a DB-FFAP (30 m × 0.25 mm, film thickness 0.25 µm, Agilent Technologies, Santa Clara, USA). An uncoated fused silica capillary was used as a pre-column (3 m × 0.53 mm) and changed regularly to avoid influences by accumulated impurities. The carrier gas was helium and the total flow was 3.3 mL/min. EI-mass spectra were generated in full scan mode (m/z range 40–400) using ionization energy of 70 eV. The starting temperature of 40 °C for the GC oven was held for 2 min, then raised at 8 °C/min to 240 °C and held for 5 min. Injection volumes were 2.0 µl.