Thermolysis of PEOM was carried out as the description by our group with some modifications (29 , 30 ). 500 mg of PEOM was put into an offline pyrolysis tank (OLT) self-made by our research group. And then, the OLT was sealed and placed in an automatic temperature-controlled electric furnace (Furnace 1,000°C, Tianjin, China) (31 ). The furnace temperature reached 100°C, and nitrogen as the carrier gas passed continuously through OLT for 10 min, meanwhile, decomposition products blown by carrier gas were absorbed by the mixture (hexane: methylene chloride: ethyl acetate = 1:1:1). Thermal decomposition products were detected by using the method of GC/MS (Agilent, Palo Alto, CA, USA). DB-5MS quartz capillary column (30 m × 0.25 mm × 0.25 μm, Agilent, USA) was used for the GC/MS analysis. Helium (99.999%) was used as carrier gas; the injector was at 250°C and the gas flow rate was set to 1.0 ml/min with splitting mode. Instrument conditions were as follows: initial temperature was set at 50°C for 3 min, then followed with a rate of 7°C/min up to 280°C, and kept for 10 min. The ion source of MS was set from 45 to 500 (m/z) with electron ionization of 70 eV. Temperature of ion source and quadrupole were 230°C and 150°C, respectively. Mass spectrometric data of constituents was retrieved from MS databases of NIST14, peak area percentage was employed to proceed with quantitative analysis.
Gc ms
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The GC-MS (Gas Chromatography-Mass Spectrometry) is a highly versatile analytical instrument used for the identification and quantification of a wide range of chemical compounds. It combines the separation capabilities of gas chromatography with the detection and identification capabilities of mass spectrometry. The GC-MS is commonly used in various fields, including environmental analysis, forensics, and pharmaceutical research, to provide detailed information about the chemical composition of samples.
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Db 5ms capillary column, by Agilent Technologies (4 mentions)
Db 5ms, by Agilent Technologies (4 mentions)
Hp 5ms column, by Agilent Technologies (3 mentions)
Masshunter software, by Agilent Technologies (3 mentions)
Db 5 capillary column, by Agilent Technologies (3 mentions)
N hexane, by Merck Group (2 mentions)
Db 5ms ui column, by Agilent Technologies (2 mentions)
Hp 5ms, by Agilent Technologies (2 mentions)
Db 5ms column, by Agilent Technologies (2 mentions)
Hplc grade dichloromethane, by Thermo Fisher Scientific (2 mentions)
Biochrom 30 amino acid analyzer, by Harvard Bioscience (2 mentions)
Ics 2000, by Thermo Fisher Scientific (2 mentions)
Icp ms, by Agilent Technologies (2 mentions)
Masshunter quantitative analysis software, by Agilent Technologies (2 mentions)
Hp msd chemstation software, by Agilent Technologies (2 mentions)
Agilent 7890 gc, by Agilent Technologies (2 mentions)
Ftir 8400s instrument, by Shimadzu (1 mentions)
Hp 5ms column, by Hewlett-Packard (1 mentions)
Lc 2010aht, by Shimadzu (1 mentions)
Atlantis hilic column, by Waters Corporation (1 mentions)
188 protocols using gc ms
1
Thermal Decomposition Analysis of PEOM
2
Metabolite Analysis of Freeze-dried Samples
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Freeze-dried samples were reconstituted in water at a volume of four times the mass of the sample, centrifuged at 16,000× g for 30 min and the supernatant transferred to a new tube. This centrifugation step was repeated twice and the extract then filtered using centrifuge filters (Merck Ultrafree-CL GV 0.22 µm). Analysis of the derivatizated compounds with methyl chloroformate was carried out by MS-Omics, Denmark, using gas chromatography coupled with a quadropole mass spectrometry detector (GC-MS, Agilent) following a slightly modified version of the method described in Smart et al. [39 (link)], and gas chromatography coupled with a quadropole mass spectrometry detector (GC-MS, Agilent). Samples were analyzed for several typical metabolite compounds from the tricarboxylic acid cycle, i.e., pyruvic acid, succinic acid, fumaric acid, malic acid, α-ketoglutaric acid, cis-aconitic acid, citric acid, isocitric acid, 4-aminobutyric acid (GABA), and malonic acid. Data were evaluated using Chemstation (Agilent) and Matlab R2018b (Mathworks Inc., Natick, MA, USA).
3
GC-MS Analysis of Yogurt Fatty Acids
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The fatty acid analysis of the yogurt samples was examined by GC-MS (Agilent Technologies Inc. Santa Clara, CA) following the method outlined by Ajmal et al. (2019) [44 (link)]. In brief, the yogurt samples were subjected to total lipid extraction using a chloroform: methanol (2:1) mixture. Subsequently, 30 μL of the extracted lipid was transferred to a 10-mL centrifuge tube, and 2 mL of hexane and benzene mixed reagent (1:1) was added and gently shaken to facilitate dissolution. Next, 2 mL of a solution containing 0.5 mol/L potassium hydroxide in methanol was added to the mixture, and the contents were shaken. The tube was allowed to stand at room temperature for 30 min, following which distilled water was added to cause the methanol solution in the organic phase to separate and rise to the top of the tube. Lastly, the supernatant was carefully extracted from the top layer after allowing the mixture to stand for 10 min in preparation for further analysis. The extracted samples were subjected to analysis using GC-MS (Agilent Technologies Inc., Santa Clara, CA, USA) with a DB5 capillary column (J&W Scientific, Agilent Technologies Inc., Santa Clara, CA, USA). The identification and quantification of individual fatty acids in the samples were accomplished by comparing their retention times and peak areas with those of corresponding standards.
4
DEHP Degradation Analysis via GC-MS
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The degradation intermediates of DEHP were detected using GC–MS (Agilent, USA) and the samples were concentrated approximately 10-fold prior to GC-MS analysis. The detection procedure conditions were set according to He [35 ] et al.
5
Characterization of Clary Sage and Black Pepper Essential Oils
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The chemical composition of clary sage and black pepper essential oil was characterised by Gas Chromatography-Mass Spectroscopy (GC-MS, Varian, Santa Clara, CA, USA). The essential oils were diluted 25 times with ethyl acetate and analysed using a Hewlett Packard mass detector and a HP-5MS column (length 30 m, inner diameter 0.25 mm, film thickness 0.25 μm). The injector, GC-MS interphase, ion source and selective mass detector temperature were maintained at 250, 280, 250 and 150 °C. The oven temperature for both oils was programmed as follows: 60 °C (1 min), 60–185 °C (1.5 °C/min), 185 °C (1 min), 185–275 °C (9 °C/min), 275 °C (2 min). Split injection was performed with helium as carrier gas, with a flow rate of 1.1602 mL/min. The split ratio of the column was fixed at 40:1. The pressure of the column was set at 9.4 psi. The components were identified by comparing the mass spectra obtained with mass spectra of standards obtained with the same column.
Fourier Transform Infrared Spectroscopy (FTIR) analysis was carried out using Attenuated Total Reflection Infrared (ATR-IR) technique (FTIR-8400S instrument, Shimadzu, Columbia, DC, USA). The range of scan was 600–2500 cm−1 with 64 scans and resolution of 4 cm−1.
Fourier Transform Infrared Spectroscopy (FTIR) analysis was carried out using Attenuated Total Reflection Infrared (ATR-IR) technique (FTIR-8400S instrument, Shimadzu, Columbia, DC, USA). The range of scan was 600–2500 cm−1 with 64 scans and resolution of 4 cm−1.
6
Biofilm Carbohydrate Analysis via GC-MS
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Samples of biofilm pellets were desiccated and subjected to methanolysis with 400 μl of acidic methanol at 80°C for 12 h to generate the methyl glycosides. Re-N-acetylation was carried out with the addition of 25 μl of acetyl chloride and 25 μl of pyridine in 150 μl of methanol for 30 min. The samples were volatilized by the addition of 50 μl of trimethylsilyl (Thermo Fisher Scientific). Samples were analyzed on a Varian GC-MS in the electron ionization mode. The monosaccharide composition was determined by comparison with known standards from Sigma-Aldrich.
7
Enzymatic Hydroxylation of n-Hexane
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Example 1
Hydroxylation of n-hexane
Enzymatic hydroxylation of hexane was performed in the pure substrate (n-hexane, >97%, Sigma Aldrich) containing 2 U ml−1 (0.31 nmol) AaeAPO added as aqueous enzyme solution (10 μl). H2O2 (4 mM) was added by syringe pumps over 1 hour. The experiment was done in 200 μl scale (total volume) in 1 ml glass vials stirred with a magnetic stirrer. Products were analyzed by GC-MS (Varian) by direct injection of the reaction mixture. Controls were processed identically except that water (10 μl) was added instead of enzyme solution.
The gas chromatogram and mass spectra of the sample with active enzyme (AaeAPO) and n-hexane showed formation of high amounts of 2-hexanol, and 3-hexanol; the control without enzyme did not contain any of these peaks.
8
Extraction and Analysis of DEET
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Reference materials, as well as influent and effluent from the reactors, were collected, placed on ice, and submitted to the Alberta Innovates Analytical Facility for extraction and determination of DEET levels. A liquid–liquid (dichloromethane) extraction method was used, and extracts were analyzed on an Ion Trap, Varian GC‐MS.
9
Enzymatic Hydroxylation of n-Hexane
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Example 1
Hydroxylation of n-hexane
Enzymatic hydroxylation of hexane was performed in the pure substrate (n-hexane, >97%, Sigma Aldrich) containing 2 U ml−1 (0.31 nmol) AaeAPO added as aqueous enzyme solution (10 μl). H2O2 (4 mM) was added by syringe pumps over 1 hour. The experiment was done in 200 μl scale (total volume) in 1 ml glass vials stirred with a magnetic stirrer. Products were analyzed by GC-MS (Varian) by direct injection of the reaction mixture. Controls were processed identically except that water (10 μl) was added instead of enzyme solution.
The gas chromatogram and mass spectra of the sample with active enzyme (AaeAPO) and n-hexane showed formation of high amounts of 2-hexanol, and 3-hexanol; the control without enzyme did not contain any of these peaks.
10
Quantification of Fatty Acid Methyl Esters
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Fatty acid methyl esters (FAMEs) were prepared according to the method previously reported by our group [19 ]. After O-methylation, the FAMEs were separated and quantified by gas chromatography-mass spectrometry (GC-MS) using an Agilent model 6890-5973 GC-MS equipped with a flame ionization detector and HP-88 fused silica capillary column (100 m × 0.25 mm i.d. × 0.2 μm film thickness). Helium was used as the carrier gas at a flow rate of 1 mL/min and the detector temperature was 250°C. The split ratio was 30 : 1 and the column temperature was programmed as follows: (i) the initial oven temperature was 80°C and it was maintained at 80°C for 5 min; (ii) the oven temperature increased to 150°C at a rate of 10°C/min and was maintained at 150°C for 2 min; (iii) the oven temperature increased to 230°C at a rate of 5°C/min and was maintained at 230°C for 10 min. The individual fatty acids were identified by comparison of the retention times with preprepared standards and quantified using an external standard. The analysis of each oil sample was conducted in triplicate, and the mean value was used for the later variance analysis.
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