For GC-MS analysis of enzyme assays, samples were injected in split mode (2 μl; split ratio, 5:1) at an inlet temperature of 220°C on a Hewlett Packard 6890 GC-MS equipped with a 5973 mass selective detector and an Agilent 7683B series injector and autosampler. Separation was performed on a Zebron ZB5-HT-INFERNO column (5% phenyl methyl siloxane; length, 35 m; diameter, 250 μm) with guard column. Helium was used as mobile phase at a constant flow rate of 1.2 ml/min and an average velocity of 37 cm/s. Two temperature runs were used for detection: Method 1 (GES, G8H, and NEPS assays): After 5 min at 80°C, the column temperature was increased to 110°C at a rate of 2.5 K/min then to 280°C at 120 K/min and kept at 280°C for another 4 min. Method 2 (HGOA assays): After an initial temperature at 60°C, the column temperature was increased to 100°C at a rate of 20 K/min then to 160°C at 2 K/min, then another increase to 280°C at 100 K/min, and maintained for 4 min. A solvent delay of 5 min was allowed before collecting MS spectra at a fragmentation energy of 70 eV. Chemically characterized standards were used to identify compounds by retention time and EI spectra.
6890 gc ms
Manufactured by Agilent Technologies
The 6890 GC-MS is a gas chromatograph-mass spectrometer system designed for analytical applications. It is capable of separating and identifying chemical compounds in complex mixtures. The system combines gas chromatography for sample separation with mass spectrometry for compound identification and quantification.
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6 protocols using 6890 gc ms
1
GC-MS Analysis of Enzyme Assays
2
GC-MS Analysis of Derivatized Samples
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GC-MS analysis was accomplished following the protocol described in Reference [51 (link)] with slight modification. The derivatized sample (µL) was injected in the splitless mode into the GC-MS system, which consisted of an Agilent 6890 GC-MS and an HP 5973 mass selective detector. The DB-5MS 5% phenyl methyl siloxane column with an inner diameter (ID) of 250 μm and a film thickness of 0.25 μm (Agilent Technologies Inc, Santa Clara, CA, USA) was used. The initial oven temperature was set to 85 °C, and then increased to a target temperature of 315 °C at a rate of 2 °C/min with a total running time of 120 min. Helium was used as the carrier gas with a flow rate of 1 mL/min. The injector and ion source temperatures were set to 250 and 280 °C, respectively. Mass spectra were acquired using a full scan and a monitoring mode with a mass scan range of 50 to 550 m/z. The spectra for each of the chromatogram peaks were compared with those in the NIST14 database library. The chromatogram and mass spectra were processed using an Agilent ChemStation, Automated Mass Spectral Deconvolution and Identification System and Agilent’s Deconvoluted Reporting Software (Agilent Technologies Inc, Santa Clara, CA, USA).
3
GC-MS Analysis of Thyme Essential Oil
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The samples of thyme EO obtained by four different extraction methods were analyzed using gas chromatography–mass spectrometry (GC–MS). The analysis was carried out on a Agilent 6890 GC–MS instrument equipped with a HP‐5MS fused silica column (30 m long, 0.25 mm i.d., 0.25 mm film thickness); Helium was used as the carrier gas at a flow rate of 0.8 mL/min with a split ratio equal to 1:50 and 1 μL of the obtained EO was injected. The injector and detector temperatures were kept at 250 and 280°C, respectively. The column temperature increased from 50 to 240°C at a rate of 3°C min−1 and from 240 to 300°C at a rate of 15°C min−1. The retention time at 50 and 300°C was 5 and 3 min, respectively. The mass ratio analyzed was 33 to 500 m z−1. The identification of compounds was based on retention times of n‐alkanes (C6–C24) that were injected after the oil at the same temperature and conditions. Compounds were identified by comparison of their RI with those reported in the literature and their mass spectrum was compared with the Wiley Library (Hudaib et al. 2002 ; Hashemi et al. 2011b ).
4
GC-MS Analysis of Organic Compounds
5
Quantification of Six Haloacetic Acids
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The six HAAs were separated and detected using gas chromatography-mass spectrometry (Agilent, 6890 GC-MS) system. Chromatographic separation was accomplished on HP-5MS 5% phenyl methyl siloxane (30 m × 0.25 mm × 0.25 mm nominal) from J&W Scientific. The column was initially maintained at 40°C for 1 min and then increased to 180°C at the rate of 25°C/min. This was held for 11 min followed by another ramping to 250°C at 30°C/min. This was maintained for 2 min. The GC-MS interface and the ion source temperatures were set at 200°C. Helium (99.999%) at a head pressure of 50 kPa was used as carrier gas with flow rate of 2.0 mL/min. The split/splitless injector temperature was set at 250°C. The injection volume was 0.2 μL and injection was performed using a 10 μL GC microsyringe.
6
GC-MS Analysis of Organic Compounds
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Samples were injected in split mode (2 μL, split ratio 20:1) at an inlet temperature of 220 °C on a Hewlett Packard 6890 GC-MS equipped with a 5973 mass selective detector (MSD), and an Agilent 7683B series injector and autosampler. Separation was performed on a Zebron ZB5-HT-INFERNO column (5% phenyl methyl siloxane; length: 35 m; diameter: 250 μm) with guard column. Helium was used as mobile phase at a constant flow rate of 1.2 mL/min and average velocity 37 cm/s. After 5 min at 80 °C, the column temperature was increased to 110 °C at a rate of 2.5 K/min, then to 280 °C at 120 K/min, and kept at 280 °C for another 4 min. A solvent delay of 5 min was allowed before collecting MS spectra at a fragmentation energy of 70 eV.
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