Lcms 2020 mass spectrometer

To assess the amount of surfactant molecules on fallen and unaffected mosquitoes after spraying, we sprayed 2 mM DOSS solution to mosquitoes flying in the mosquito net at a distance of 40 cm and collected 7 unaffected and 6 fallen mosquitoes. The mosquitoes were stored individually in screw-top glass vials (Maruemu Corporation) in the fridge until extraction. We added 1 mL of 50% methanol (Kanto chemical Co., Inc.) solution to the vials and extracted DOSS on mosquito body by vigorously vortexing them for 1 min. DOSS on mosquito body was quantified by high-performance liquid chromatography coupled to mass spectroscopy using LCMS2020 (Mass spectrometer; Shimadzu). The injection volume was 5 μL for each sample solution. L-column2 ODS (3 μm, 2.1 × 150 mm, Chemicals evaluation and research institute) was used as the analysis column. The HPLC solvent consisted of solvent A (50% methanol containing 100 mM ammonium acetate) and solvent B (95% methanol containing 100 mM ammonium acetate). The samples were separated with a linear gradient from 50 to 100% solvent B with a low rate of 300 nL/min using HPLC. The mass spectrometer was operated in a selected ion monitoring (SIM) mode with m/z 421.20 for DOSS. Calibration lines were generated by plotting the concentration against the peak area of DOSS.

The fungal strain Fusarium verticillioides (MRC 826) was inoculated on pre-soaked, sterile maize kernels, in a form of spore suspension. The incubation was set to 25 °C for 5 weeks, and the final FBs concentration in dried culture material was harvested in different production batches. Details on fungal culture preparation were published earlier [72 (link)]. The final FB₁ concentrations were 2000–4000 mg/kg in the air-dried culture material harvested in different batches. The FB₂ concentration of the inoculum materials was ca. 30% of the FB₁ content and the FB₃ concentration was ca. 10–15% of the FB₁ content. The fungal culture was mixed into the ration of the experimental animals so as to provide a daily FBs (FB₁ + FB₂ + FB₃) feed concentration of 15 and 30 mg/kg. The diet fed to the control group did not contain detectable amounts of FBs, whereas the experimental diets were mixed with fungal culture to provide 15 and 30 mg FBs/kg diet. In the diets, the absence of FBs co-occurrence with deoxynivalenol (DON), zearalenone (ZEN), and T-2 toxin was also confirmed, in which the analyzed diets did not contain detectable concentrations (below the limit of detection; 0.053, 0.005, and 0.011 mg/kg for DON, ZEN, and T-2 toxin, respectively). The content of FBs was determined by the LC-MS-2020 mass spectrometer (Shimadzu, Kyoto, Japan) [73 (link)].

All commercial reagents and solvents
were used as-received without further purification. Reactions were
monitored via thin-layer chromatography performed on Merck silica
gel plates (60 F254) or analytical liquid chromatography/mass spectroscopy
(LC/MS) performed on a Shimadzu Shim-pack XR-ODS (C18, 2.2 μm,
3.0 × 50 mm, linear gradient from 10% to 100% B over 3 min, then
100% B for 1 min [A = water + 0.1% formic acid, B = MeCN + 0.1% formic
acid], flow rate: 1.6 mL/min) using a Shimadzu UFLC system equipped
with a LCMS-2020 mass spectrometer, LC-20AD binary gradient module,
SPD-M20A photodiode array detector (detection at 254 nm), and SIL-20AC
sample manager. All compounds used in the bioassay are >95% pure
as
determined by HPLC analysis. Flash column chromatography was performed
on an automated purification system using Fuji Silysia prepacked silica
gel columns. ¹H and ¹³C NMR spectra were recorded
on a Bruker Advance at 400 and 100 MHz, respectively. Spectral data
are reported as follows: chemical shift (as ppm referenced to tetramethylsilane),
integration value, multiplicity (s = singlet, d = doublet, t = triplet,
q = quartet, m = multiplet, br = broad), and coupling constant. High-resolution
mass spectra were recorded on a Thermo Fisher Scientific LTQ Orbitrap
using electrospray positive ionization.

Unless otherwise noted, the following instruments and conditions were used. The ¹H-NMR, ¹³C-NMR, and 2D-NMR spectra were recorded using an ECA-800 or ECA-600 spectrometer (JEOL), and chemical shifts were expressed in δ (ppm) with tetramethylsilane (TMS) as the reference standard. The LC/Orbitrap MS analysis was performed using an LC-20A UFLC system (Shimadzu) equipped with the LTQ Orbitrap XL mass spectrometer (Thermo Fisher Scientific). The UPLC/MS analysis was performed using a Xevo TQD UPLC/MS system (Waters). The LC/MS analysis was performed using an LC-20A UFLC system equipped with an LCMS-2020 mass spectrometer (Shimadzu).

An aqueous solution of CV/MB/RhB dyes mixtures were prepared (5 ppm). 80 mg of as-prepared CuS nanoparticles were added into 50 mL of dyes mixture. The suspension was stirred in a dark condition for 45 min. Afterward, the suspension was exposed to mercury lamp visible light (70 W). A UV-visible spectrophotometer was used to measure the absorbance of the photo irradiated suspension. The initial dyes and degraded intermediate products were detected through Shimadzu LCMS-2020 mass spectrometer (Kyoto, Japan).

LC/MS measurements were carried out using an Orbitrap Exploris 240 mass spectrometer at 60,000 resolution (Thermo Fisher Scientific) for confirmation of peptides in the venom and an LCMS-2020 mass spectrometer (Shimadzu, Kyoto, Japan) for confirmation of peptide synthesis. For analysis by Orbitrap Exploris 240, an RP-HPLC column (Everest C18 1.0 mm × 250 mm, Hichrom, Reading, UK) was used for separation; this column was eluted with 0.1% formic acid in H₂O (solvent A) and 0.1% formic acid in CH₃CN (solvent B) at a flow rate of 0.05 mL/min using a linear gradient of 5–50% of solvent B over 45 min. For analysis by LCMS-2020, an RP-HPLC column (Poroshell 120-EC-C18 2.1 mm × 75 mm, Agilent) was used for separation; this column was eluted with 0.1% formic acid in H₂O (solvent A), and 0.1% formic acid in CH₃CN (solvent B) at a flow rate of 0.3 mL/min using a linear gradient of 5–60% of solvent B over 15 min.