J w vf 5ms column

A Trace GC Ultra instrument (Thermo Fisher Scientific) was used with helium as carrier gas, in programmable temperature vaporization splitless injection mode at a flow rate of 1.5 mL/min. Injector temperature was 250 °C and a volume of 1 µL was injected. The instrument was equipped with a J&W VF-5MS column (45 m × 0.32-mm i.d., film thickness 0.4 µm, Agilent Technologies). The GC temperature program was as follows: time (min)/oven temperature (°C) 0/40, 1/40, 10/130, 15/280 and 20/280. The GC was coupled to a TSQ Quantum mass spectrometer (Thermo Fisher Scientific) operating in MRM mode in positive polarity with an electron energy of 70 eV. The solvent delay time was 4 min. Precursor ions were fragmented using argon as collision gas and a collision energy of 10 eV with monitoring transitions from m/z 125 to 99 and from m/z 99 to 81.

The GC-MS system used comprised of a Gerstel 2.5.2 autosampler, a 7890A Agilent gas chromatograph and a 5975C Agilent quadrupole mass spectrometer (Agilent, Santa Clara, CA, United States). The mass spectrometer was tuned according to the manufacturer’s recommendations using tris-(perfluorobutyl)-amine (CF43).
Gas chromatography was performed on a 30 m Agilent J & W VF-5MS column with 0.25 μm film thickness and 0.25 mm internal diameter with a 10 m Integra guard column. The injection temperature (Inlet) was set at 250°C, the MS transfer line at 280°C, the ion source adjusted to 230°C, and the quadrupole at 150°C. He was used as the carrier gas at a flow rate of 1 mL min^–1.
The analysis of TMS-derivatized samples was performed under the following temperature program; start at injection 70°C, a hold for 1 min, followed by a 7°C min^–1 oven temperature ramp to 325°C and a final 6 min heating at 325°C. Mass spectra were recorded at 2.66 scans.s^–1 with an 50–600 m/z scanning range.

An Agilent 6890 gas chromatograph (GC) (Agilent Technologies, Wilmington, CA, USA) with a mass detector (MS) was used to measure the samples. The MS detector was heated to 230 °C. An Agilent J&W VF-5 ms column (5% phenyl and 95% dimethylpolysiloxane) with 30 m × 0.25 mm i.d., with a diameter of 0.25 m, was used. The oven heating cycle started at 200 °C for 4 min, rose to 280 °C at a rate of 10 °C min⁻¹, and remained there for 7 min. Helium, at 1.0 mL min⁻¹, was the carrier gas (99.996%). The injection system was in splitless mode. One µL of the sample was injected. The GC-MS apparatus was operated and the data were processed with Chemstation software. With these chromatographic parameters, it was possible to obtain a retention time (T_r) of 7.5 min for erucamide.