Trace 1300-TSQ 9000 GC-MS (Thermo Scientific, Waltham, MA, USA) equipped with a VF-WAX-MS capillary column (30.0 m × 0.25 mm × 0.25 μm, Agilent, Santa Clara, CA, USA) was applied to detect the volatile flavors of the PM [20 (link)]. Briefly, 1.00 g APM and 20 μL methyl octanoate (internal standard, 0.0079 g/100 mL) were accurately added to a 20 mL headspace bottle, and a 50/30 μm DVB/CAR/PDMS fiber (2 cm, Supelco, Bellefonte, PA, USA) was used to extract volatile flavors at 60 °C for 50 min, and then, the extraction head was removed and inserted into the inlet and desorbed for 5 min. The GC conditions were as follows: inlet temperature, 270 °C; carrier gas, high-purity helium (>99.999%); flow rate, 1 mL/min; spitless. The temperature of the column was as follows: 40 °C for 5 min, 4 °C/min to 100 °C, and 6 °C/min to 230 °C for 10 min. The MS conditions were as follows: ion source temperature, 250 °C; transmission line temperature, 300 °C; ionization mode, EI (70 eV); scan range, 35–400 amu. After comparing with the NIST 2017 library, only compounds with similarity (SI) >800 remained for further analysis (the highest value is 1000). All the samples were measured in triplicate.
Vf waxms capillary column
Manufactured by Agilent Technologies
Sourced in United States
The VF-WAXms capillary column is a high-performance analytical column designed for gas chromatography (GC) applications. It features a stationary phase of polyethylene glycol (PEG) and is intended for the separation and analysis of a wide range of polar and semi-polar compounds.
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4 protocols using vf waxms capillary column
1
GC-MS Analysis of Volatile Flavors
2
Terpene Identification in Patchouli Oil
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Terpene
products were identified by analyzing samples with a gas chromatographer
coupled with a mass spectra detector (Agilent 7890B system), equipped
with a 30 m VF-WAXms capillary column (0.25 mm I.D. × 0.25 μm
thickness, Agilent). Samples of 0.5 μL were injected into the
device using on-column mode with the following oven program: 40 °C
for 3 min, 10 °C per min to 230 °C increase and 10 min final
hold. Additional settings included 1 mL per min of constant gas flow
(helium 5.0); 230 °C for the ion source; 150 °C for the
quadrupole, 33–300 m/z for
the mass scan range, and 70.0 eV for the ionization energy. Identification
of terpene products was performed by comparing retention indices and
mass spectra of samples with references from the mass spectral NIST
14 database and authentic standards obtained from the patchouli oil
(Sigma-Aldrich W283800), extracted from P. cablin (Blanco) Benth of Indonesia.
products were identified by analyzing samples with a gas chromatographer
coupled with a mass spectra detector (Agilent 7890B system), equipped
with a 30 m VF-WAXms capillary column (0.25 mm I.D. × 0.25 μm
thickness, Agilent). Samples of 0.5 μL were injected into the
device using on-column mode with the following oven program: 40 °C
for 3 min, 10 °C per min to 230 °C increase and 10 min final
hold. Additional settings included 1 mL per min of constant gas flow
(helium 5.0); 230 °C for the ion source; 150 °C for the
quadrupole, 33–300 m/z for
the mass scan range, and 70.0 eV for the ionization energy. Identification
of terpene products was performed by comparing retention indices and
mass spectra of samples with references from the mass spectral NIST
14 database and authentic standards obtained from the patchouli oil
(Sigma-Aldrich W283800), extracted from P. cablin (Blanco) Benth of Indonesia.
3
GC-MS Analysis of Volatile Organic Compounds
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VOCs were identified using a 7890B & 5977A Series GC/MSD (Agilent Technologies, Santa Clara, CA, USA), where chromatographic separation was achieved on a VF-WAXms capillary column (30 m × 0.25 mm × 0.25 µm; Agilent Technologies, Santa Clara, CA, USA). The overall temperature program was as follows: 40 °C (1 min) to 60 °C at 5 °C min−1 (held 1 min), then to 100 °C at 7 °C min−1, to 180 °C at 10 °C min−1 and finally to 200 °C at 15 °C min−1 (held 1 min). The carrier gas was helium at a constant flow of 1.5 mL min−1. The injection was performed at 250 °C in the split mode (1:10), using a Straight Ultra Inert Liner for SPME (Agilent Technologies, Santa Clara, CA, USA). The ion source was set to 230 °C and the interface temperature to 250 °C, with a scan range of 30 to 400 m/z. The system was controlled using the ChemStation software (Agilent Technologies, Santa Clara, CA, USA). The identification procedure was performed by comparing retention times and mass spectra with the NIST 14 Mass Spectral Library (Agilent Technologies, Santa Clara, CA, USA) and pure standards.
4
Comprehensive GC-MS Analysis of FAMEs
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Analysis was carried out using a 7890B GC and 5977A Series GC/MSD (Agilent, Santa Clara, CA, USA). Separation was achieved on a 30 m × 0.25 mm × 0.25 μm VF-WAXms capillary column (Agilent J&W, Santa Clara, CA, USA). The injection volume was 1 μL, with a split ratio of 10:1. The carrier gas was helium maintained at a 1.5 mL/min constant flow. The injector temperature was 280 °C and the detector temperature 350 °C. The temperature program was as follows: initial column temperature set at 50 °C for 1 min then programmed to 170 °C at 15 °C/min and held for 5 min, then from 170 °C to 200 °C at 3 °C/min, held 5 min, and from 200 °C to 230 °C at 5 °C/min, and held 17 min.
A standard Supelco 37 component FAME Mix in dichloromethane (Bellefonte, PA, USA) was used for identification and quantification. Compounds were identified based on a comparison of retention times with authentic compounds. With each set of samples, blank samples and the FAME Mix standard were analyzed to verify the stability of the analytical system. The results are expressed as the weight percent of an individual fatty acid to the total fatty acid (TFA) content calculated from the peak area using the appropriate correction factors [30 ].
A standard Supelco 37 component FAME Mix in dichloromethane (Bellefonte, PA, USA) was used for identification and quantification. Compounds were identified based on a comparison of retention times with authentic compounds. With each set of samples, blank samples and the FAME Mix standard were analyzed to verify the stability of the analytical system. The results are expressed as the weight percent of an individual fatty acid to the total fatty acid (TFA) content calculated from the peak area using the appropriate correction factors [30 ].
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