GC-MS analyses were performed by using a HP 6890 Series Plus gas chromatograph (Agilent Technologies, Palo Alto, CA, USA) equipped with a MSD 5973 mass spectrometer (Agilent Technologies, Palo Alto, CA, USA). The following operating conditions were applied: carrier gas—helium—at a constant flow rate of 1.2 mL/min; GC injector: splitless mode at 260 °C; chromatographic separation on a Rxi-5Sil MS capillary column (30 m × 0.25 mm i.d., 0.25 μm film thickness; Restek, Bellafonte, USA), applying the following temperature program: 90 °C hold for 2 min, 15 °C/min to 180 °C, 20 °C/min to 270 °C; transfer line and ion source at 280 °C and 150 °C, respectively. Full-scan EI data were acquired to determine appropriate m/z ion ratios for time scheduled monitoring using the following conditions: ionization energy: 70 eV; mass range: 50–350 amu; scan time: 3 scan/s; electron multiplier voltage: 1000 V, solvent delay 2.00 min. All the analyses were carried out by operating in selected ion monitoring mode (SIM), dwell time 30 ms, monitoring the following ions: m/z 74 , 143 and 186 for methyl decanoate; m/z 69 , 114 and 250 for methyl farnesoate (ions used for quantitation in bold). Signal acquisition and data handling were performed using the HP Chemstation (Agilent Technologies).
Rxi 5sil ms capillary column
Manufactured by Restek
Sourced in United States
The Rxi-5Sil MS capillary column is a high-performance fused silica column designed for gas chromatography-mass spectrometry (GC-MS) applications. It features a 5% diphenyl-95% dimethyl polysiloxane stationary phase that provides effective separation of a wide range of analytes, including polar and nonpolar compounds. The column is inert and thermally stable, making it suitable for a variety of GC-MS analyses.
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Lab products found in correlation
5973 msd mass spectrometer, by Agilent Technologies (1 mentions)
Hp chemstation, by Agilent Technologies (1 mentions)
Tsq 8000 triple quadrupole mass spectrometer, by Thermo Fisher Scientific (1 mentions)
Triplus ai 1310 autosampler, by Thermo Fisher Scientific (1 mentions)
Pegasus ht, by Leco (1 mentions)
Trace gc ultra, by Thermo Fisher Scientific (1 mentions)
Quantum xls mass spectrometer, by Thermo Fisher Scientific (1 mentions)
Rxi 17, by Restek (1 mentions)
Agilent 7890a gc, by Agilent Technologies (1 mentions)
Multipurpose sampler, by Gerstel (1 mentions)
Gcms qp2010, by Shimadzu (1 mentions)
Agilent 5975, by Agilent Technologies (1 mentions)
Db wax capillary column, by Agilent Technologies (1 mentions)
6890 gas chromatograph, by Agilent Technologies (1 mentions)
Pegasus 4d tofms, by Leco (1 mentions)
7890a gc system, by Agilent Technologies (1 mentions)
Agilent 7890 m780ei gas chromatograph, by Agilent Technologies (1 mentions)
Chromatof software, by Leco (1 mentions)
Vf 5ms capillary column, by Agilent Technologies (1 mentions)
7890b gas chromatograph, by Leco (1 mentions)
15 protocols using rxi 5sil ms capillary column
1
GC-MS Analysis of Methyl Esters
2
GC-MS/MS Analysis of Pesticide Residues
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The analytes were detected by Thermo Scientific TSQ8000 triple quadrupole mass spectrometer with a Trace 1310 gas chromatograph and a TriPlus AI 1310 autosampler (Thermo Fisher Scientific, San Jose, CA). The chromatographic separation column was a Rxi®-5Sil MS capillary column (20 m × 0.18 mm, 0.18 μm film thickness) (Restek, USA). The temperature program of the column was 40 °C (held for 0.6 min), increased to 180 °C at 30 °C min−1, then ramped to 280 °C at 10 °C min−1, finally up to 290 °C at 20 °C min−1 and held for 5 min. The injection port temperature was 250 °C, and the injection volume was 1 μL in splitless mode. Argon was selected as collision gas, and helium gas (99.999% purity) was used as carrier gas with a constant flow of 0.85 mL min−1. The temperature of transfer line to tandem MS and ion source all was 280 °C. The triple quadrupole MS was operated in electron ionization (EI) mode with the electron energy of 70 eV. The selected reaction monitoring (SRM) was used as an acquisition mode. The retention time, ion pair, and collision energy (CE) of each pesticide were shown in Table S1 in ESI.† 18 (link)
3
GC-TOF/MS Analysis of Metabolites
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The GC-TOF/MS analysis was performed using an Agilent 7890 gas chromatograph system coupled with a Pegasus HT time-of-flight mass spectrometer (LECO Chroma TOF Pegasus HT, LECO, Saint Joseph, MI, USA), which utilized a Rxi-5Sil MS capillary column coated with 5% diphenyl cross-linked with 95% dimethylpolysiloxane (30 m × 250 μm inner diameter, 0.25 μm film thickness; Restek, Bellefonte, PA, USA). A 1-μL aliquot of the analyte was injected in the splitless mode, and helium was used as the carrier gas, with a 3 mL/min front inlet purge flow and 1 mL/min gas flow rate through the column. The initial temperature of the column was maintained at 50 °C for 1 min; then, it was raised to 330 °C at a rate of 10 °C/min and maintained for 5 min. The temperatures for the injection, transfer line and ion source were 280, 280, and 220 °C, respectively. The mass spectrometry data were acquired using a mass-to-charge ratio (m/z) range of 85–600 at a rate of 20 spectra per second after a solvent delay of 366 s in the full-scan mode with electron impact ionization at 70 eV. The stability of the injected sample was tested by evaluating the retention time (RT) of the internal standard.
4
Quantitative Analysis of Methyl Salicylate in Wine
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Analysis of free methyl salicylate was performed using a Trace GC Ultra gas chromatograph coupled to a Quantum XLS mass spectrometer (Thermo Scientific, Austin, TX, USA) mounted with a PAL combi-xt autosampler (CTC, Zwingen, Switzerland). A Rxi®-5Sil MS capillary column (30 m × 0.25 mm × 0.25 μm, Restek Corp. Bellefonte, PA) was used. One microliter of sample was injected in splitless mode with a GC inlet temperature of 250 °C. Helium was used as a carrier gas in constant flow mode at 1.2 mL/min. The oven temperature was programmed as follows: (i) initial temperature 50 °C held for 2 min, (ii) linearly raised by 8 °C/min to 150 °C, and (iii) in the final step, the temperature was ramped at 20 °C/min to 280 °C, and maintained for 1 min (total run-time was 22 min). The mass spectrometer was operated in positive electron ionization mode at 70 eV and all spectra were recorded in full scan with a mass range of 40–350 Da; transfer line and source temperatures were set at 250 °C. Electron ionization was applied at 70 eV with an emission current of 50 μA. Thermo Excalibur software (1.1.1.03, Thermo Scientific, Waltham, MA, USA) was used for all acquisition control and data processing. A calibration curve was generated, spiking the model wine solution with 5–500 μg/L of methyl salicylate.
5
Serum Metabolite Profiling by GCxGC-TOFMS
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Pegasus GCxGC-TOFMS (Leco Corporation Joseph, MI, USA) that uses an Agilent 7890A GC (Atlanta, GA) coupled to a time-of-flight mass spectrometer (TOFMS) (Leco Corporation, St Joseph, MI, USA) equipped with a Gerstel Multipurpose sampler, was used for chromatographic analyses of the derivatized samples. One µL of serum extract was randomly injected at a split ratio of 1:50 and the carrier gas used was helium at a flow rate of 1 ml min−1. For the entire run, the temperature of the injectors was kept constant at 270°C. A Restek Rxi-5Sil MS capillary column (29.145 m × 0.25 μm d.f.) was used as the primary column. The primary oven was programmed to an initial temperature of 70°C for 2 min to obtain a compound separation. Subsequently, this was followed by a 4°C per minute increase to a final temperature of 300°C where it was maintained for 2 min. The second separation of compounds was achieved using a Restek Rxi-17 (1.400 m, 0.25 µm i.d., 0.25 μm d.f.) column. The secondary column used was set to the same temperature parameters as that of the primary column. The filament bias was EI at 70 eV while the detector voltage was at 1,600 V. Subsequently, the mass spectra were collected at an acquisition rate of 200 spectra per second with a source temperature of 220°C and a solvent delay of 400 s from 50 to 800 m/z (Du Preez and Loots 2013 (link)).
6
Gas Chromatography-Mass Spectrometry Olfactory Analysis
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Odor analyses were carried out on a GCMS-QP2010 (Shimadzu, Tokyo, Japan) equipped with a thermal desorption TD 20 (Shimadzu, Tokyo, Japan) and coupled to the olfactory detection port (Phaser, GL Sciences, Holland). The olfactometer consisted of a glass cone purged with air previously humidified by passing through a bubbler containing water. A calculation program (Split Manager Software) calculated all flows, and split the ratio between the nose and the detector. The volatile compounds were simultaneously detected by MS and sniffing after 1:1 splitting of the eluate at the column outlet. Analyses were performed on a Restek RXI -5Sil MS capillary column (30 m × 0.25 mm ID × 0.25 µm df).
7
GC-MS Analysis of Organic Compounds
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The GC-MS system and the analytical conditions were the same as those in our previous paper53 (link). GC separation was achieved on a Restek Rxi®-5Sil MS capillary column (30 m, inner diameter 0.25 mm and film thickness 0.25 µm). The oven temperature was programmed at 50 °C for 5 min, increased at 3 °C/min to 210 °C, then increased at 15 °C/min to 330 °C and kept for a 5 min final hold. The MS was operated in an electron impact (EI) mode with ionization energy of 70 eV and a mass scan range of 30–500 m/z. Samples were analyzed in triplicates. QC samples prepared by pooling aliquots of all samples were injected every ten runs throughout the analysis to monitor instrument fluctuations.
8
GC-O-MS Analysis of Tomato-Onion Extract
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The gas chromatography-olfactometry-mass spectrometry (GC-O-MS) system consisted of an Agilent 6850 gas chromatograph coupled with an Agilent 5975 mass selective detector (Agilent, Santa Clara, CA, USA), an Olfactory Detection Port (ODP-2) and a MPS-2 as autosampler (Gerstel, Mulheim, Germany).
Chromatographic separations were conducted on two different columns: Rxi-5-Sil MS capillary column (30 m × 0.25 mm × 0.25 μm, Restek Corporation, Bellefonte, PA) and DB-WAX capillary column (20 m × 0.18 mm i.d., 0.3 μm film thickness; Agilent Technologies J&W, Santa Clara, CA, USA), with helium as carrier gas at 1.25 mL/min flow.
The liquid extracts (1µL) were injected in splitless mode. The injector was equipped with a Cooled Injection System (CIS). The GC effluent was split 1:1 into the MS and the sniffing port (ODP-2). The oven temperature was programmed starting from a temperature of 35 °C, which was retained for 2 min, following increase of 5 °C/min to 230 °C.
Mass spectra in the electron impact mode (MS-EI) were generated at 70 eV and they were taken over the m/z range 33 and 300 m/z with a speed of 2.7 scan/s and with a solvent delay of In order to determine the odour-active molecules, a GC-O analysis was performed on the tomato-onion extract by using a detection frequency method (section 2.3.3) and an aroma extract dilution analysis (AEDA) (section 2.3.4).
Chromatographic separations were conducted on two different columns: Rxi-5-Sil MS capillary column (30 m × 0.25 mm × 0.25 μm, Restek Corporation, Bellefonte, PA) and DB-WAX capillary column (20 m × 0.18 mm i.d., 0.3 μm film thickness; Agilent Technologies J&W, Santa Clara, CA, USA), with helium as carrier gas at 1.25 mL/min flow.
The liquid extracts (1µL) were injected in splitless mode. The injector was equipped with a Cooled Injection System (CIS). The GC effluent was split 1:1 into the MS and the sniffing port (ODP-2). The oven temperature was programmed starting from a temperature of 35 °C, which was retained for 2 min, following increase of 5 °C/min to 230 °C.
Mass spectra in the electron impact mode (MS-EI) were generated at 70 eV and they were taken over the m/z range 33 and 300 m/z with a speed of 2.7 scan/s and with a solvent delay of In order to determine the odour-active molecules, a GC-O analysis was performed on the tomato-onion extract by using a detection frequency method (section 2.3.3) and an aroma extract dilution analysis (AEDA) (section 2.3.4).
9
GC-TOF-MS Metabolomic Analysis Protocol
10
GC-FID Analysis of Cycloartenol and 24-Methylcycloartenol Derivatives
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(CA+24-MCA) (2 mg) was derivatized to trimethylsilyl ethers by adding 300 μL N,O-bis(trimethylsilyl) trifluoroacetamide and 50 μL pyridine at 60°C for 30 min. Cycloartenol (CA) standard (2 mg) was also derivatized using the same protocol. TLC/HPTLC profiling showed complete conversion of (CA+24-MCA) and standard CA into their trimethylsilyl derivatives. Derivatives of (CA+24-MCA) and standard CA were dissolved in 1.5 mL chloroform and 1 μl each were injected (splitless) on a Gas Chromatograph with AOC-20i autoinjector and FID (GC-2010 Plus, Shimadzu, Japan), fitted with a Rxi-5 Sil MS capillary column (5% phenyl 95% dimethyl polysiloxane, non-polar, 30 m x 0.25 mm i.d., 0.25 μm film thickness (Restek, USA). GC operation conditions: injector temperature 270°C; GC oven was initially maintained at 50°C (2 min), oven temperature programme: 50–280°C (10°C/min), hold time at 280°C (30 min) and FID was set at 280°C. Carrier gas nitrogen, flow rate 1.53 mL/min. GC analyses of samples were repeated four times each and relative percentages of individual components (derivatives of CA, 24-MCA) were calculated from the peak area-percent report of the GC-FID data.
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