6850 gas chromatograph

IR spectra were recorded on a Perkin Elmer (Model: Spectrum BX) FT-IR spectrometer using CHCl 3 . All 1 H and 13 C spectra were recorded on 300 MHz (Brucker) and 500 MHz (Varian) spectrometers, respectively. HRMS data were recorded on a Thermo Scientific Exactive Orbitrap mass spectrometer (Germany) and are given in mass units (m/z) . ESI-MS spectra were recorded on Waters (Model: Q STAR XL, Applied Biosystems, USA) Mass Spectrometer equipped with an Electrospray Ionization source. Elemental analyses were carried out by using Elementar Vario Micro Cube instrument (Germany) . Gas chromatography was performed on an Agilent 6850 gas chromatograph equipped with a flame ionization detector. The column used was a HP-1 column having a length of 30 m, 0.25 mm i.d and 0.25 μm film thickness. The carrier gas was nitrogen at a flow rate of 1 mL・min -1 . The oven programming was as follows: 150℃ for 2 minutes, which rose to 300℃ at a rate of 10℃ min -1 and held at 300℃ for 20 minutes. The injector and detector temperatures were maintained at 280 and 300℃ respectively.

The derivatized samples were analyzed with a Hewlett Packard 6850 Gas Chromatograph, 5973 mass selective detector, and 7683B series injector (Agilent Technologies, Palo Alto, CA), using helium as the carrier gas at 1.0 mL•min -1 flow. One microliter of sample was injected in the split-less mode and resolved on a 30 m × 0.25 mm × 0.25 µm DB-5MS column (Agilent Technologies). Inlet, interface, and ion source temperatures were 250, 250, and 230°C, respectively. Oven starting temperature was set to 50°C, final temperature to 230°C with a heating rate of 5°C min -1 for 36 min and then for 2 min at constant temperature. Electron impact mass spectra were recorded from m/z 50 to 550 at 70 eV. The resulting data were analyzed using MSD ChemStation software (Agilent Technologies). The identification of metabolites was performed by comparison with instrumental analytical standards injected database and by metabolite mass spectra comparison with the NIST14 library of the National Institute of Standards and Technology (Gaithersburg, MD). The GC-MS spectra deconvolution was performed through NIST14 library's AMDIS tool. For each metabolite, the GC-MS peak area related to the most abundant and representative mass fragment was calculated using MSD ChemStation software.

Analyses of FAME were carried out by using an Agilent Technologies Inc. 6850 gas chromatograph (Milan, Italy), equipped with a split-splitless injector, a FID detector and a column MegaWax 25 m long, ID 0.32 mm, film thickness 0.25 μm (Mega s.n.c, Legnano, Italy). Analytical conditions are as follows: oven temperature from 40 °C (initial time 1 min) to 150 °C (10 °C/min), to 250 °C (5 °C/min) (final time 5 min); H 2 as carrier gas (flow rate 1.2 mL/min); injection temperature 300 °C; volume injected 1 μL and split ratio 1:50. Peak areas were determined by means of Software Agilent G2070 ChemStation.