The GC-MS analyses of Ormenis eriolepis Dichloromethane Fraction (Oe-DF) and Hexanic Extract (Oe-HE) were carried out at the Instrumental Technical Services of the “Estación Experimental del Zaidín” (CSIC, Granada, Spain). Briefly, 1 μl of the derivative solution was injected in a Varian 450GC coupled to 240 Ion Trap Mass Spectrometer as detector. The injection conditions were: splitless mode with 1 minute duration pulse, the injector temperature was 250°C; the He column flow was 1 ml/minute in a capillary column (Varian Factor Four VF-5 ms 30mx0.25mmx0.25 pm). For Mass spectrometry conditions, the EI ionization was 70 eV, the transfer line was at 280°C and the Trap at 240°C, mass range acquisition was from m/z 50 to m/z 500 and cared in Full Scan mode. Qualitative analysis of compounds was based on the comparison of their spectral mass and their relative Retention time with those of NIST08 mass spectra database and Kovats RI on the chromatograms recorded in Full Scan or in SIM mode usin g the characteristics ions. Quantitative analysis was realized by integration of peaks and calculated as percent of total identified area on the TIC chromatograms.
Factorfour vf 5ms
Manufactured by Agilent Technologies
The FactorFour VF-5ms is a capillary gas chromatography column designed for the separation and analysis of a wide range of volatile organic compounds. It features a 5% phenyl-methylpolysiloxane stationary phase and measures 30 meters in length with a 0.25 millimeter internal diameter and a 0.25 micrometer film thickness.
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6 protocols using factorfour vf 5ms
1
GC-MS Analysis of Ormenis eriolepis Fractions
2
Phytosterol Characterization by GC-MS
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Samples were prepared for GC-MS (gas chromatography and mass spectrometry) analysis by adding 5 μL of pyrinde and 5 μL of BSTA to dry phytosterol samples. The samples were vortexed for 15 s and 40 μL of chloroform was added. The solution was transferred to a 50 μL GC vial and 1 μL was injected into the GC-MS (Agilent GC 6890N gas chromatograph fitted with a 7683B Automatic Liquid Sampler and a 5975B Inert MSD quadrupole MS detector (Agilent Technologies). The capillary column on the gas chromatograph was 0.25 mm (i.d.) with a 0.25 µm film thickness, and 30 m Varian FactorFour VF-5ms and was fitted with a 10 m integrated guard column (Varian). The inlet temperature was constant at 300 °C. The helium carrier gas flowed at a constant rate of 1 mL min−1. The GC oven temperature was set at 100 °C initially for 1 min with an increase to 320 °C at a rate of 37 °C min−1 and then held for 2 min. The transfer accession temperature was set at 280 °C, MS source at 230 °C, and quadrupole temperature at 150 °C. Ionization was by electron impact at 70 eV. The mass calibrant perfluorotributylamine was used to pre-tune the MS. Data analysis was performed through Agilent GC/MSD Productivity Chemstation software. The phytosterols were identified by comparing their retention times and mass to that of the internal standard.
3
Gas Chromatography Analysis of Essential Oils
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EO samples were analysed and the relative peak areas for individual constituents were averaged. The relative percentages were determined using a ThermoQuest GC-Trace gas-chromatograph equipped with a FID detector and a Varian FactorFour VF-5ms poly-5% phenyl-95%-dimethyl-siloxane bonded phase column (i.d., 0.25 mm; length, 30 m; film thickness, 0.25 µm). Operating conditions were as follows: injector temperature 280 °C; FID temperature 300 °C, carrier gas (Helium) flow rate 1 mL/min and split ratio 1:50. Oven temperature was initially 55 °C and then raised to 90 °C at a rate of 1 °C/min, then raised to 250 °C at a rate of 10 °C/min and finally held at that temperature for 15 min. Each sample was dissolved in CH2Cl2 (1:100 v/v) and 1 μL was injected. The percentage composition of the EOs was computed by the normalisation method from the GC peak areas, calculated by means of three injections from each EO, without using correction factors.
4
GC-MS Analysis of Organic Compounds
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Electron impact (EI) analyses were conducted using a Varian 431-GC instrument with a capillary column Factor Four™ VF-5ms (30 m × 0.25 mm × 0.25 μm) and a Varian 210-MS ion trap mass detector. Scans were performed from 40 to 650 m/z at rate of 1 scan per second. The oven temperature program applied during the analysis was: initial temperature 95 °C, hold for 1 min, ramp at 15 °C min−1 to 200 °C, hold for 2 min., ramp at 15 °C min−1 to 300 °C, hold for 5 min. The injector transfer line temperature was set to 250 °C. Measurements were performed in the split–split mode (split ratio 50 : 1) using helium as carrier gas (flow rate 1.0 mL min−1).
5
GC-MS Analysis of Organic Compounds
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A Varian 431 GC instrument with a capillary column FactorFourTM VF-5 ms (30 m·0.25 mm·0.25 μm) and a Varian 210 ion trap mass detector were used. Scans were performed from 40 to 650 m/z at rate of 1.0 scans·s−1. The oven temperature program was: initial temperature 95 °C, hold for 1 min, ramp at 15 °C·min−1 to 200 °C, hold for 2 min, ramp at 15 °C·min−1 to 325 °C, hold for 5 min. Measurements were performed in split–split mode (split ratio 50:1) using helium as the carrier gas (flow rate 1.0 mL·min−1).
6
GC-MS Analysis of Wine Volatiles
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All analyses were carried out on a Varian Saturn 2000 (Varian, Inc., Walnut Creek, CA, USA) GC-MS system composed by a Star GC 3400 CX (Varian, Inc.) gas chromatograph connected to an ion-trap mass detector. The GC apparatus was equipped with a 1078 split/splitless injector with a SPME liner inside. All injections were performed in a split mode with a 50:1 split ratio. A Varian FactorFourTM VF5-ms (Varian, Inc.) capillary column (30 m × 0.25 mm × 0.25 µm film thickness) was used and the carrier gas was Helium IP, supplied at a flow rate of 1.0 mL/min. The column oven temperature program was the following: initial temperature 35 °C for 5 min, then raised at 5 °C/min to 150 °C and held for 1 min, and finally increased to 280 °C with at a rate of 10 °/min and held for 5 min. Retention indices of the extracted compounds were determined on the basis of the observed retention times of aliphatic hydrocarbons (C7-C24). These data were collected by HS-SPME/GC-MS analysis of the Retention Index Standard after dilution with a water-ethanol mixture, under application of the same temperature program used in the analysis of wine volatiles.
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