Gcms2010 plus

NMR spectra were recorded on a Bruker 400 MHz spectrometer in CDCl₃ with tetramethylsilane (TMS) as the interval standard. Matrix Assisted Laser Desorption Ionization (coupled to a Time-Of-Flight analyzer) experiments (MALDI-TOF) was recorded on a Shimadzu GCMS 2010 PLUS. Thermogravimetric analyses (TGA) measurements were conducted by a Shimadzu DTG-60H under a heating rate of 10^oC min^–1 and a nitrogen flow rate of 50 cm³ min^–1. Differential scanning calorimetry (DSC) measurements were performed using a Shimadzu Instruments DSC-60A and DSC data were collected from 30 to 200 ^oC at a rate of 10 ^oC min^–1 under N₂ flow.

Byproduct analysis was performed as described previously [30 (link)]. Acetone (900 μL) was added to 100 µL of liquid fraction and mixed thoroughly. The sample was then centrifuged at 21,880×g and room temperature for 10 min. The supernatant (10 µL) was subjected to GC–MS analysis (GC-MS-2010plus; Shimadzu). 5-HMF and furfural were analyzed under the following conditions: column, Agilent CP-Sil 8CB-MS (30 m × 0.25 mm); carrier gas, helium; injection temperature, 250 °C; oven temperature, 50 °C at t = 0–5 min, then increased to 280 °C at 20 °C/min. Acetic acid and formic acid were analyzed under the following conditions: column, Agilent DB-FFAP (60 m × 0.25 mm); carrier gas, helium; injection temperature, 250 °C; oven temperature, 100 °C at t = 0 to 5 min, then increased to 230 °C at 10 °C/min.

Gas chromatography-flame ionization detection and gas chromatography–mass spectrometry analyses were accomplished with Shimadzu QP2010 Plus and GCMS2010 Plus (Shimadzu Corporation, Kyoto, Japan) systems. The GC-MS and GC-FID conditions and the identification of the chemical constituents of the EOs were carried out in agreement with the methodology proposed by Santos et al. [43 (link)].

CZ-EO was dissolved in ethyl ether and analyzed by gas chromatography flame- ionization detection (GC-FID) and gas chromatography-mass spectrometry (GC–MS) on the Shimadzu QP5000 Plus and GCMS2010 Plus (Shimadzu Corporation, Kyoto, Japan) systems, respectively. During GC-FID, the column temperature was programmed to rise from 60 to 240 °C at 3 °C/min and held at 240 °C for 5 min. H₂ was used as the carrier gas at a flow rate of 1.0 mL/min. The equipment was set to operate in the injection mode; the injection volume was 0.1 µL (split ratio of 1:10); and the injector and detector temperatures were 240 and 280 °C, respectively. Relative concentrations of the CZ-EO compounds were estimated from the relative peak areas (%) of the GC-FID chromatograms, and expressed as the average of triplicate analyses and the corresponding standard deviations. GC-MS conditions and the identification were based on a previously reported methodology [17 (link)]. The volatile components in CZ-EO (Table 1) were identified on the basis of their retention indices on an Rtx-5MS (30 m × 0.25 mm; 0.250 µm) capillary column, under the same operating conditions used for the GC relative to a homologous series of n-alkanes (C₈–C₂₀). The structures were computer matched with Wiley 7, NIST 08, and FFNSC 1.2, and their fragmentation patterns were compared with literature data [21 ].

Aroma analysis of roasted Tan mutton was performed by a GC-MS system (GC-MS 2010 plus, SHIMADZU, Japan) jointed with solid-phase microextraction (SPME) fiber. Briefly, 2 ± 0.01 g of the sample after crushed were placed into a 15 mL headspace bottle with 4 μL of internal standard (1,2-dichlorobenzene, 6.42 μg/mL in methanol). After mixing with a vortex, the headspace bottle was sealed with a PTFE diaphragm, and placed in a water bath at 55°C for 20 min. The aged SPME fiber (50/30 μm DVB / CAR / PDMS) was inserted into a sealed extraction bottle and kept on the top of the mutton sample for adsorption for 30 min, and then transferred to the GC inlet for desorption at 250°C for 5 min. The chromatographic capillary column was DB-WAX (30 m × 0.25 mm × 0.25 μm, Agilent Technologies, Santa Clara, CA). The GC and MS were carried out in accordance with our previous study (25 (link)).

For GC-MS analyses, 2 × 10⁶ HuH7 cells were scraped in 400 μL ice-cold water to be then supplemented with 400 μL methanol and 500 μL chloroform. After vigorous vortexing, samples were centrifuged at 10,000× g for 10 min at 4 °C. Organic phases were collected and dried. Sample was solubilized in pyridine (50 μL) and derivatized with 25 μL of N,O-Bis(trimethylsilyl(TMS)trifluoroacetamide with trimethylchlorosilane (BSTFA+TMS) with a reaction time of 90 min. GC-MS analyses were carried out on a Shimadzu GCMS 2010plus (Kyoto, Japan) with the following parameters. Injection temperature 280 °C, Ramp 0–1.00 min 100 °C, 1.00–6.00 min 100–320 °C, hold for 2.33 min, column flow 1.10 mL/min, linear velocity 39 cm/s. Helium gas was used. Ion source temperature 200 °C, Interface 320 °C, Solvent cut 5.9 min, Scan 35–600 m/z. Detector voltage 0.1 kV. Separation was performed on an Agilent (Santa Clara, CA, USA) SIL-8, 30 m by 0.25 mm, 0.25 μm. Then, 1 μL was injected, split ratio 1:10.

GC-MS analysis was done according to method described by Yong et al. [4 (link)]. Crude extract of plant sample was analysed with gas chromatography equipped with mass spectrometry (GC-MS-2010 Plus-Shimadzu). The column temperature was set to 50°C for 4 min before it was increased to 320°C at the rate of 7°C/min and was then held for 20 min. The injector temperature was set at 280°C (split mode with the ratio being adjusted to 20 : 1, injection volume = 0.1 µL). The flow rate of the helium carrier gas was set to 1 mL/min with total run time of 60 min. Mass spectra were obtained from the range m/z 40 to 700 and the electron ionization at 70 eV. The chromatogram of the sample was identified by comparing their mass spectra with the library data and the GC retention time against known standards.