Qp2010 gc ms system

The gas chromatographic and mass spectroscopic (GC-MS) analysis of the rose oil extracted from fresh petals of Rosa damascena was executed by a QP2010 GC-MS system (Shimadzu, Tokyo, Japan) which was coupled with an AOC-5000 auto-injector, and DB-5 (SGE International, Ringwood, Australia) fused silica capillary column (30 m × 0.25 mm and a film thickness 0.25 μm). The programmed temperature was from 70 to 220°C (4 and 5 min) with a stepwise increase in temperature at the rate of 4°C min⁻¹ for 5 min; the injector temperature was 240°C and interface temperature was 250°C, respectively. The ionization voltage used was 70 eV with 800–50 amu acquisition mass range, and the carrier gas used was helium, whose flow rate was 1.1 ml per min. Homologous series of n-alkanes (C8–C24) was used to calculate the retention indices (RI) of all volatile components. Then, for the identification of rose oil compounds, the calculated values of retention indices (RI) and their mass spectra were matched with the database of the NIST-MS library (Stein, 2005 ). After that, the quantification was completed by GC analyses.

The volatile components were analyzed using a Shimadzu QP 2010 GC-MS system equipped with an AOC-20i Autosampler. Chromatographic separation was performed on a DB-5 MS column (0.25 μm ×0.25 mm ×30 m). The temperature program was set as follows: 40°C for 0 min, 40–190°C in increments of 7°C/min, 190–230°C in increments of 2°C/min, and 230°C for 1 min.
Mass spectrometry was performed in electron impact (EI) mode and full scan mode at m/z 50–1,000. The temperatures of ion source and interface were 230 and 250°C, respectively. The detector voltage was 1.3 kV.

For the gas chromatography–mass spectrum (GC–MS) analysis, tissue samples were mixed with 600 µl methanol/water (v/v 4:1) solution containing internal standards followed by thorough homogenization in a mixed grinding apparatus (MM400, Retsch, Germany) at 25 Hz for 2 min. Supernatants were lyophilized for subsequent oximation and silylation reactions. A QP 2010 GC–MS system (Shimadzu, Japan) with a DB-5 MS fused-silica capillary column (30 m × 0.25 mm × 0.25 µm, Agilent Technologies, Santa Clara, CA, USA) was used for the metabolic profiling. A pseudotargeted GC–MS metabolomics method was established elsewhere [11 (link)–13 (link)]. A total of 280 ion features assigned to 23 groups were defined for the data collection and quantification. The system parameter settings were previously described [13 (link)]. Metabolite identities were determined based on commercial libraries (Mainlib, NIST, Wiley, and Fiehn) and an internal metabolite library.

The extraction and sample preparation of CR dye metabolites after PUF-immobilized microbial consortium treatment under upflow column bioreactor conditions was carried out [21 (link)]. For this, the treated dye samples were collected and suspended solids were removed by centrifugation (10,000× g for 15 min, 4 ± 0.2 °C). This resulted clear supernatant was extracted thrice with an equal volume of ethyl acetate, organic layer collected and dried in a SpeedVac (Thermo Fisher Scientific Inc., Waltham, MA, USA). It was then dissolved in methanol, filtered through 0.45 µm pore size cellulose acetate filters and subjected to HPLC (Agilent 1200 series HPLC system, Agilent Technologies, Santa Clara, CA, USA), FTIR (Nicolet iS 10 spectrometer, Thermo Fisher Scientific Inc., Waltham, MA, USA) and GC-MS (QP2010 GC-MS system, Shimadzu Corporation, Kyoto, Japan) analysis as per an earlier report [22 (link)]. CR dye (100 mg·L⁻¹) was dissolved in methanol and analyzed to obtain control spectra.

Shimadzu QP-2010 GC-MS system equipped with a capillary column (inner diameter 0.25 mm and length 30 m) was used to analyse the constituents of the EtOH extract of R. officinalis [15 (link)]. The temperature of the GC oven was kept at 100 °C for two minutes and was further programmed to 280 °C at the rate of 10 °C/min and then kept at 280°C for 13 min. The split ratio was 1: 25 and the injection volume was 2 μL. The injection port and detector port temperatures were 200°C and 240°C, respectively. The GC-MS electron ionization mode was 150 eV. The mass scanned was between m/z 20–500 amu (70 ms accumulation time). The peaks of the gas chromatogram were subjected to mass spectral analysis. The active constituents were identified based on the retention indices and by the comparison of mass spectra with the National Institute of Standards and Technology library of mass spectral data.

AIR (1.5 mg) was pyrolyzed in an EGA/PY-3030D pyrolyzer (Frontier Laboratories, Saikon Koriyama, Japan) connected to a QP2010 GC/MS system (Shimadzu, Kyoto, Japan) with a DB-5 capillary column (30 mm × 0.25 mm × 0.25 μm, Agilent, Santa Clara, CA, USA). The pyrolysis was heated from 200 °C (maintained for 1 min) to 600 °C (maintained for 10 s), and the rate of temperature rise was 20 °C/min. The GC was heated from 40 to 280 °C, the rate of temperature rise was 5 °C/min, and maintained 10 min at 280 °C. The flow rate of helium was 2 mL/min. The results were identified for compensation according to the standards of the Wiley and National Institute of Standards and Technology (NIST) libraries [17 (link)]. Finally, the peak area was calculated and normalized.
The composition results of straw by pyGC-MS include carbohydrate related (C), guaiacyl units (G), syringyl units (S), and p-hydroxyphenol units (H). The generic benzene derivatives, which without OH group on the aromatic ring (but most probably originated from lignin related compounds) (P), a substance that knows spectra information (unknown identification) (U) and unknown spectra (cannot be lignin or carbohydrates) (0), also were determined. Each substance was expressed as a percentage of the total (C+G+S+H+P+U+0). The total lignin refers to G+S+H+P.

The collected fecal sample (100 mg) was homogenized in methanol (1 ml) by vigorous vortex for 3 min and sonicated for 10 min. The mixture was then centrifuged at 4°C (14000 rpm, 5 min) to obtain the supernatant, which was further diluted by 5-folds with methanol. The diluted supernatant (0.5 ml) was mixed with trimethyl acetic acid (internal standard, 5 μg/ml) solution (0.5 ml) and followed by injecting the mixture (1 μL) into Shimadzu QP2010 GC-MS system (Tokyo, Japan) for analysis. The analysis was carried out on an Agilent J & W fused silica capillary column (0.25 μm, 30 m) and the instrument parameters were set according to the reported method with modifications (Tsang et al., 2018 (link)). Briefly, the transfer line temperature and ion source temperature were 230°C and 200°C, respectively. High purity helium served as the carrier gas. The ionization mode was electron impact, with the electron energy of -70 eV and scanning time of 0.5 s. Mass fragments (m/z) in the range of 10–650 were monitored and identified in NIST Mass Spectral Library.