Qp2010 plus gc ms system

PSO (5 g) was hydrolyzed with 20 mL of 2 M KOH in methanol at 60°C for 30 min. The unsaponifiable fraction was extracted using the method of Wang et al. [17 ]; meanwhile, the saponifiable fraction was converted to fatty acid methyl esters (FAMEs) and extracted into hexane according to the method of Zhou et al. [9 ]. For both fractions, the residues were dried under vacuum and weighed after the extraction solvents were removed. The percentage weight of unsaponifiable matters (R_um) and fatty acids (R_fa) in PSO was calculated as W_uf/W_oil × 100% and (1 − W_uf/W_oil) × 100%, respectively, where W_uf meant the weight of unsaponifiable fraction and W_oil the weight of PSO. Then both residues were redissolved in hexane and subjected to analysis by gas chromatography-mass spectrometry (GC-MS) using a Shimadzu QP2010 Plus GC-MS system (Kyoto, Japan) according to conditions previously reported [9 , 17 ]. Qualitative analysis was conducted by matching peak mass fragmentation patterns with those in NIST05 mass spectrum libraries, and quantitative analysis was carried out by normalizing peak areas to obtain the percentage content of each component, P_ep, from which its rate in PSO (R) could be calculated by multiplying with R_um or R_fa.

Gas Chromatography-Mass Spectrometry (GC-MS) analysis was employed to characterize and quantify bioactive substances in the seaweed extracts. Methanolic extracts were characterized quantitatively via GC-MS, according to slight modifications to the method adopted by Han et al. 2009 [21 (link)], using a Shimadzu QP2010 Plus GC-MS system. In the experimental procedure, 0.5 μL of the sample was separated on a Zebron ZB5-ms 30 m × 0.25 mm ID x 0.25 μm film thickness) column. The splitless injection was performed using a purge time of 1 min. Helium represented the carrier gas at a flow rate of 1 mL/min. The column temperature was maintained at 50°C for 3 min, then programmed at 250°C for 10 min, and maintained at 250°C for 30 min. The inlet and the detector temperatures were set at 250°C, and the solvent cut time was set at 4.50 min. The identification of peaks was based on a computer-based program matching the mass spectra with those in the library for the National Institute of Standards and Technology (NlST3208 and NIST 08s). This was done by comparing retention time data with that obtained for authentic laboratory standards. Individually detected peak areas were quantified and expressed as a percentage of total components detected.

GC analyses were carried out on a Shimadzu 2010 GC-FID system and a Shimadzu QP2010 plus GC-MS system, provided with an AOC-20i automatic injector. Data were processed with Shimadzu GC Solution 2.53SU1 software and Shimadzu1224 PGCMS Solution 2.51 software, respectively (Shimadzu, Milan, Italy).
GC-FID-MS analyses were carried out on a Mega 5 column (95% polydimethyl-siloxane, 5% phenyl) 25 m×0.25 mm dc ×0.25 μm df, from MEGA (Milan, Italy).
Analysis conditions were as follows: injection mode: split; split ratio: 1:20; injection volume: 1 μl. Temperatures: injector:250°C, FID: detector: 280°C, MS: transfer line:280°C; ion source: 200°C; carrier gas: He, initial flow rate 1.0 ml/min in constant linear velocity mode. The temperature programme was from 50°C (1 min) to 250°C (10 min) at 3°C/min (5°C/min for Mega-Dex DMT-Beta column). The MS was operated in electron impact ionization mode at70 eV, with a mass range of 35–350 m/z in full scan mode.
EO components were identified by comparison of both their linear retention indices (I^Ts), calculated versus a C9-C25 hydrocarbon mixture, and their mass spectra to those of authentic samples, or to those reported in commercially available mass spectral libraries [22 ].

Serum was thawed on the ice, and a 50 μL of blood sample was drawn and mixed with 200 μL of methanol containing ISs (Supplemental Table s1). As previously described, supernatants were lyophilization-treated for subsequent oximation and silylation reactions [16 (link)]. Then, the supernatant was obtained for GC-MS analysis. A QP 2010 Plus GC-MS system (Shimadzu, Japan) with a DB-5MS (Agilent Technologies, USA) was used. A QC sample was inserted for every 10 samples to evaluate the data quality. The instrument and procedure of GC-MS analysis were described in the previous study [16 (link)].

The GC-MS experiment was performed using a QP 2010Plus GC-MS system equipped with an AOC-20i auto-sampler (Shimadzu, Kyoto, Japan). The system utilized a DB-5 ms fused-silica capillary column (30 m × 250 μm × 0.25 μm, J&W Scientific, Folsom, CA). The interface and ion source temperatures were set to 320 °C and 230 °C, respectively. High-purity helium was used as the carrier gas at a constant linear velocity of 40.0 cm/s. The initial oven temperature was 80 °C for 1 min, ramped to 210 °C at 30 °C/min, increased to 320 °C at 20 °C/min, and maintained for 4 min. An electron ionization source was used, and the ionization voltage was set to 70 eV. The mass scan range was 33–600 m/z, and the solvent delay was 2.92 min.