Qp2010 se gc ms

A Shimadzu QP 2010-SE GCMS coupled to an auto sampler was used for the analysis. Ultrapure Helium was used as the carrier gas at a flow rate of 1 ml/minute. A BPX5 non polar column, 30 m; 0.25 mm ID; 0.25 μm film thickness, was used for separation. The GC was programmed as follows: 50⁰ C (1 min); 30⁰ C /min to 300⁰ C. Only 1 μL of the sample was injected. Injection was done at 200⁰ C in split mode, with split ratio set to 10:1. The interface temperature was set at 280⁰ C. The Electron Ionisation (EI) ion source was set at 200⁰ C. Mass analyses was done in Single Ion Monitoring (SIM) mode at specific retention windows. SIM group ions for permethrin were 127, 163 and 183 m/z; with 183 m/z being the quantifier ion. The retention window for these ions was between 24 and 26 min. SIM group ions for α-cypermethrin were 127, 163 and 181; with 163 m/z being the quantifier ion. The retention window for these ions was between 26.5–28.5 min. To test the method suitability, extraction efficiency (Additional files 3, 4, 5, 6 and 7), repeatability (Additional files 8, 9, and 10), accuracy and limit of detection (Additional file 11), were determined before sample injection. All samples were analysed at the Jomo Kenyatta University of Agriculture and Technology (JKUAT) analytical chemistry laboratory.

The liquid product mixture after the reaction
was analyzed on a Shimadzu QP2010 SE GC–MS apparatus, equipped
with an RTX-1701 column (60 m × 0.25 mm ID × 0.25 μm),
and a flame ionization detector (FID) together with a mass spectrometer
detector. GCMSsolution and GCsolution software were used for the analysis.
Products in the liquid phase were identified based on a search of
the MS spectra in the NIST11 and NIST11s MS libraries. The quantitative
analysis of the liquid phase products was based on the GC-FID measurements.
The FID weight response factors of all product compounds in the liquid
mixture were determined using the Effective Carbon Number (ECN) concept
relative to n-dodecane as the internal standard.
The yields of monomers, oligomers, and char were determined according
to eqs 1–3: Char yield
is defined as a
combination of THF-insoluble lignin fragments and actual char, as
was collected during the workup procedure after step (6) (Figure 2).

The GC-MS analysis of the hexane extracts of A. greatheadii was conducted using a SHIMADZU QP2010 SE GC-MS with an inert cap 5MS/SIL, silica capillary column (30 mm × 0.25 mm ID X 1 µmdf, composed of 100% dimethyl-poly-siloxane). An electron ionization system with an ionizing energy of 70 eV was used for detection. Helium gas (99.99%) was used as the carrier gas at a constant flow rate of 1 mm/min with an injection volume of 2 ul; injector temperature of 290°C; and ion-source temperature of 230°C. The oven temperature was set from 50°C (isothermal for 1 min), with an increase of 20°C/min to 180°C (isothermal for 5 min), and then increased to 240 C at 20°C/min, ending with an increase of 20ºC/min to 280°C (isothermal for 5 min). Mass spectra were taken at 70 eV; scan interval of 0.3 sec; and fragments from 50 to 700 m/z [8 ]. The software adopted to handle the mass spectra and chromatogram was GC-MS Solutions version 2.6. Identification of compounds was based on the mass spectra from the GC-MS and was performed using the compound database of the National Institute of Standard and Technology (NIST08) library. The mass spectra of unknown compounds were compared with those of components stored in the NIST08 library with the hit of 90% and above regarded as a positive match. The retention time, name, molecular weight, and molecular formula of the identified compounds were recorded.

Glassware and amber bottles were cleaned with phosphate-free soap bought from Dynachem (Durban, South Africa) and were left in the acid bath for a day. Then all glassware (Searle, Vervaardig, South Africa) were further washed with 5% dichloromethylsilane, finally rinsed with methanol, and then placed in the oven (Prolab, Durban, South Africa) at 60 °C for 12 h. Micro-volumes were transferred by a micropipette plus kit bought from Dragon lab (Beijing, China) ranging between 0.5 to 1000 μL. All glass fibre filters were purchased from Pall Corporation (Johannesburg, South Africa). Extraction cartridges (Oasis HLB 20 cc (1 g and 60 mg) LP, tC18 environmental cartridge sepak-pak and sepak-pak plus CN cartridge) were bought through Microsep (Durban, South Africa), a local supplier of Waters Corporation (Milford, MA, USA) products in South Africa. A Shimadzu QP2010 SE GC-MS (Kyoto, Japan) equipped with an autosampler and autoinjector (AOC-20i) (AOC-20s) was used for analysis. The capillary column, Crossbond 5% diphenyl/95% dimethyl polysiloxane (intercap 5 Sil MS 0.25 mmL. D χ 30 M df = 0.25 μm, non-polar) purchased from Restek (Bellefonte, PA, USA) was used for GC separation. Experiments were conducted at a room temperature of 20 °C.

Phytosterols were analyzed using QP2010 SE GC-MS (Shimadzu, Tokyo, Japan) after silylation with trimethylsiloxy groups [−O-Si(CH₃)₃; TMS] group. The analytical details are summarized in Table 3. The mass fragmentation pattern of obtained phytosterols was compared with authentic standards and reference databases, including Wiley9, NIST08, and NIST08S.

A fraction of the prepared cinnamon extract was dissolved in hexane (0.05 mg/mL) and analyzed using QP2010 SE GC-MS (Shimadzu, Tokyo, Japan). The analytical conditions are listed in Table 1. Quantitative analysis was performed using a calibration curve (0.1–0.01 mg/mL) with a trans-cinnamaldehyde standard (Merck, Rahway, NJ, USA) as per the protocol described by Wang et al. [53 (link)].