Analyses were performed using a gas chromatographer (PerkinElmer, model Auto System XL, CA, USA) and a RTX-5MS WCOT capillary column (Restek, 30 m × 0.25 mm; film thickness 0.25 µm) coupled to a quadrupole mass spectrometer (PerkinElmer, model Turbo PE Turbomass-Gold, San Jose, CA, USA). Helium was used as a carrier gas at 1.00 mL L−1, in the split mode with a split ratio of 1:30. Mass spectra were obtained in El mode (70 eV) and scanned from m/z 45 to 650. The sample injection was done in an initial oven temperature of 60 °C for 1 min, raised to 100 °C at 7 °C min−1 and then to 300 °C at a rate of 4 °C min−1, and held for 10 min. The GC-MS analyze was made in duplicate for each sample, and the compound identification by chromatograms were made according to the NIST database.
Rtx 5ms wcot capillary column
Manufactured by Restek
Sourced in United States
The RTX-5MS WCOT capillary column is a fused silica column with a 5% diphenyl-95% dimethyl polysiloxane stationary phase. It is designed for a wide range of analyte separations, including polycyclic aromatic hydrocarbons, pesticides, and other organic compounds.
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4 protocols using rtx 5ms wcot capillary column
1
GC-MS Analysis of Chemical Compounds
2
GC-MS Analysis of Chemical Compounds
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Samples were analyzed by quadrupole type GC–MS system composed by an Agilent 7683B Series Injector coupled to an Agilent HP6890 Series gas chromatograph system and a 5973 Mass Selective Detector. The GC separation was performed with RTX-5MS WCOT capillary column (Restek, 30 m × 0.25 mm; film thickness, 0.25 mm), by applying a 2 minutes long isothermal phase at 80°C, followed by a temperature increase from 80 to 310°C (rate of 15°C min-1) and culminating in a 10 minutes long isothermal phase at 310°C. The helium gas was set at 1 mL min−1, while the injector temperature at 250°C and the split flow was 25 mL min−1. Mass spectra were obtained in EI mode by scanning in the range from 50 to 650 m/z, with a cycle time of 0.2 scan s−1. The compounds identification was carried out by the mass comparison with real standard or with the mass spectra libraries of both NIST 05 (http://www.nist.gov ) and Max-Planck-Institute for Plant Physiology of Golm (Germany, http://csbdb.mpimp-golm.mpg.de/csbdb/dbma/msri.html .
3
Offline TMAH Thermochemolysis of Humic Substances
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For the offline TMAH analysis, 500 mg of dried HS sample were weighed in a quartz boat and treated with 1 mL of TMAH (25% in methanol) solution. After one night, the mixture was dried under N 2 , introduced into a Pyrex tubular reactor (50 cm × 3.5 cm i.d.) and heated at 400 °C for 30 min in a round horizontal furnace (Barnstead Thermolyne). The molecular components released by thermochemolysis were conveyed by a helium flow (20 mL min -1 ) into two chloroform (50 mL) solutions kept into an ice/salt baths. After pyrolysis, the solutions were combined and dried by roto-evaporation. The residue was redissolved in 1 mL of chloroform and transferred in a glass vial for GC-MS analysis. The GC-MS analyses were conducted with a Perkin Elmer Autosystem XL equipped with an RTX-5MS WCOT capillary column (Restek, 30 m × 0.25 mm; film thickness, 0.25 μm), coupled, to a PE Turbomass-Gold quadrupole mass spectrometer. The chromatographic separation was achieved by the following parameters: injector temperature = 250 °C, with split-injection mode (30 mL min -1 of split flow); oven program = 60 °C (1 min isothermal), rate 7 °C min -1 to 320 °C (10 min isothermal); carrier gas (He) flow = 1.90 mL min -1 . Mass spectra were obtained in EI mode (70 eV), by scanning in the range 45-650 m/z with a cycle time of 1 s.
4
GC-MS Characterization of Essential Oils
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The chemical characterization of EOs obtained from steam distillation, was carried out by Gas Chromatography Mass Spectrometry (GC-MS) by a PE Autosystem XL Turbomass Gold mass spectrometer. The GC separation was performed with an RTX-5MS WCOT capillary column (Restek, 30 m × 0.25 mm; film thickness, 0.25 mm) and by the following operating conditions: injector temperatures 250° in split mode (30 mL min -1 ); oven program: initial temperature 60 °C/5 min, ramp 1 = 4 °C min -1 to 160 °C, ramp 2 = 15 °C min -1 to 240 °C, ramp 3 = 10 °C min -1 to a final isothermal step at 300 °C for 10 min. C. Helium (1.0 mL min -1 ) was used as a carrier gas. Mass spectra were obtained in electron ionization mode at 70 eV, scanning in the range included within 50 and 650 m/z, with a scan cycle rate of 0.2 s -1 . The chromatographic peaks were integrated by a manual mode and the identification was based on the comparison of mass spectra with the NIST-library database and published spectra.
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