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Gcms qp2010 mass spectrometer

Manufactured by Shimadzu
Sourced in Japan, Germany

The GCMS-QP2010 is a gas chromatograph-mass spectrometer (GC-MS) instrument manufactured by Shimadzu. It is designed to perform qualitative and quantitative analysis of complex organic and inorganic compounds. The core function of the GCMS-QP2010 is to separate, identify, and quantify the components of a sample mixture through the combination of gas chromatography and mass spectrometry techniques.

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13 protocols using gcms qp2010 mass spectrometer

1

Photoreaction Characterization Techniques

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The solvents were used without further purification. Pyrrolidine was previously distilled. Other commercially available materials were used as received. The photoreactions were monitored using Shimadzu GC-MSQP2010 mass spectrometer and thin layer chromatography. The TLC was carried out on Merck silica gel (60 F254) and flash chromatography was performed in silica gel (230–400 mesh). The NMR spectra were recorded on 400 MHz and 500 MHz spectrometer Varian Inova 400, Varian Inova 500 and Bruker Avance 400. Chemical shifts (δ) are expressed in ppm downfield from tetramethylsilane (TMS) as internal standard. Hydrogen coupling patterns are described as singlet (s), doublet (d), double doublet (dd), double triplet (dt), triplet (t), double quartet (dq), quartet (q), multiplet (m). Coupling constants (J) are reported in Hertz. Low-resolution mass spectra were obtained with a Shimadzu GC-MSQP2010 mass spectrometer. GC analysis were conducted on a RESTEC HP-5MS capillary column (30 m, 0.25 mm id, 0.25 μm film thickness) using the products dissolved in ethyl acetate. High-resolution mass spectra were obtained in a Micromass Q-Tof micro mass spectrometer.
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2

Pectoralis major fatty acid analysis

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Pectoralis major was minced before the chemical analysis. The extraction of lipids for fatty acid analysis was performed with chloroform/methanol (2:1 v/v) as described by Pérez-Palacios et al. [36 (link)]. Further analysis was performed following the procedures outlined in Klupsaite et al. [35 (link)]. A GC-2010 Plus gas chromatograph (Shimadzu Corporation, Kyoto, Japan) together with a GCMS-QP2010 mass spectrometer (Shimadzu Corporation, Kyoto, Japan) were used to analyze the fatty acid composition. A calibration curve was used to measure the concentration of fatty acid methyl esters (FAME), and the results were represented as a percentage of the total concentration of FAME in the sample.
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3

Analytical Characterization of Organic Compounds

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The reactions were monitored by TLC carried out on Merck silica gel (60 F254, Darmstadt, Germany) by using UV light as visualizing agent, KMnO4 in water, phosphomolybdic acid in ethanol and ninhydrine in ethanol and heat as developing agents. Column chromatography was performed using Merck Silica Gel 60. Proton nuclear magnetic resonance spectra (1H-NMR) were obtained at 400 MHz on Bruker 400 spectrometers (Billerica, MA, USA). Spectra were recorded in CDCl3, MeOD and DMSO-d6 solutions. Chemical shifts are reported in ppm, referenced to tetramethylsilane (TMS) as the external reference. Carbon-13 nuclear magnetic resonance spectra (13C-NMR) were obtained at 100 MHz on Bruker 400 spectrometer. Chemical shifts are reported in ppm, referenced to the solvent peak of CDCl3. Low-resolution mass spectra were obtained with a Shimadzu GC-MS-QP2010 mass spectrometer (Kyoto, Japan). High resolution mass spectra (HRMS) were recorded on Q Executive Plus LC-MS/MS system (Thermo Scientific, Waltham, MA, USA).
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4

VOC Profiling of T. atroviride Strains

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The profiles of VOCs produced by T. atroviride strains were performed as previously described by Nieto-Jacobo et al. (2017) (link), which were based on gas chromatography coupled to Shimadzu GCMS-QP2010 mass spectrometer (Shimadzu™ Co., Japan), and equipped with a Restek Rxi-5 ms fused silica capillary column (30.0 m x 0.25 mm id x 0.25 μm, Bellefonte, PA, USA).
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5

Synthesis of Chalcogen-Containing Heterocycles

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The reactions were monitored by thin layer chromatography (TLC), which were performed using Merck (Merck, Darmstadt, Germany) silica gel (60 F254), with a 0.25 mm thickness. For visualization, TLC plates were either exposed to UV light, or stained with iodine vapor or in a 5% vanillin solution in 10% aqueous H2SO4 and heat. Column chromatography was performed using Merck Silica Gel (230–400 mesh). High-resolution mass spectra (HRMS) were recorded in positive ion mode (ESI) using a Bruker microQTOF spectrometer (Bruker, Billerica, MA, USA). Low-resolution mass spectra were obtained with a Shimadzu GC-MS-QP2010 mass spectrometer (Shimadzu Corporation, Kyoto, Japan). NMR spectra were recorded with Bruker DPX (Bruker). (1H-NMR = 400 and 500 MHz; 13C-NMR = 100 and 126 MHz) instruments using CDCl3 as solvent and calibrated using tetramethylsilane (TMS) as internal standard. Coupling constants (J) were reported in Hertz and chemical shifts (δ) in ppm. The NMR spectra are found in the Supplementary Materials. The reagents (substituted alkynes, sodium tetrahydroborate, elemental chalcogen) and PEG-400 were purchased from Sigma-Aldrich (Sigma-Aldrich, St. Louis, MO, USA).
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6

Preparation and Characterization of Compound 1

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Precoated silica gel 60G F254 plates (Merck, Mumbai, India) were utilized for analytical and preparative thin layer chromatography (TLC). Chemline CL726 melting point apparatus was used for measurement of melting point in an open capillary tube and are uncorrected. The IR spectra (vmax, cm−1) were recorded in KBr on Shimadzu FT-IR 157 spectrophotometer. 1H and 13C NMR (d, ppm) spectra were recorded in DMSO-d6 on Bruker advance III NMR spectrophotometer operating at 500 and 125 MHz respectively and chemical shifts are reported in ppm with respect to tetramethylsilane as internal standard; coupling constants (J values) are given in Hertz. Mass spectra were determined on Shimadzu GC-MSQP 2010 mass spectrometer. Elemental analysis was performed with Elementar Vario EL III analyzer for C, H, N. Commercially available reagents and solvents (LR grade) were used without purification. Compound 1 was prepared according to the reported method.[14 ]
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7

Prodrug Structural Characterization

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The structure of the synthesized prodrugs were confirmed by differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FTIR), 1H NMR and mass spectrometry (MS). The thermal behavior of each prodrug was analyzed by a differential scanning calorimeter (Mettler Toledo, DSC822e, Switzerland). Samples (5 mg) were placed in an aluminum crucible and heated at a scanning rate of 10 °C min−1 from 25 to 400 °C under nitrogen atmosphere. For FTIR analysis, samples and potassium bromide (1 : 100) were mixed uniformly and then analyzed by a FTIR-8400s infrared spectrophotometer (Shimadzu, Japan). The 1H NMR (in DMSO-d6) spectrum of each sample was recorded on a Varian 400 spectrometer (Varian, USA) at 400 MHz using tetramethylsilane (TMS) as internal standard. The MS analysis was performed by a GCMS-QP2010 mass spectrometer (Shimadzu, Japan) equipped with an electrospray ionization (ESI) system.
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8

Synthesis and Characterization of Novel Organic Compounds

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All chemicals, solvents, and media were purchased from Sigma Aldrich, combi-block, enamine, Himedia, SRL. All purchased chemicals were used without further purification, reactions were continuously monitored by thin layer chromatography (TLC) on silica gel-(G60 F254, Merck) of 0.5 mm thickness, visualizing with ultraviolet light (254 and 365 nm), or with iodine vapour or aq KMnO 4 . Melting points were determined using a Buchi B-540 capillary apparatus. NMR spectra were recorded on a Bruker Advance 400 MHz spectrometer (400 MHz for 1 H NMR and 101 MHz for 13 C NMR) respectively in solvents like CDCl 3 , DMSO and chemical shifts were referenced to the solvent residual signals with respect to tetramethylsilane. Standard abbreviations are used to represent signals multiplicities for 1 H NMR spectrum s -singlet, d -doublet, t -triplet, qquartet, m -multiplate. The reaction temperature was monitored by ruby thermometer. Mass spectra were recorded on a Shimadzu GC-MS-QP-2010 mass spectrometer in EI (70eV) model using direct inlet probe technique and m/z were reported in atomic units per elementary charge.
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9

GC-MS Analysis of Labeled Glucose

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GC-MS was conducted with a GCMS-QP2010 plus with an AOC-20s autosampler and column inserted into the ion source of a GCMS-QP2010 mass spectrometer (Shimadzu Corporation, Kyoto, Japan). The GC was equipped with a 30 m × 0.25 mm SH-Rtx-5MS column with 0.25 μm thickness (Shimadzu Corporation). Helium at a linear velocity of 36.8 cm/s was used as the carrier gas. The injector was used in the split mode, and its temperature was kept at 250°C. The GC column temperature was programmed to increase 80 to 320°C at a rate of 15°C/min. Retention time for the derivatives of [U-12 C]-glucose and [U-13 C]-glucose were around 13 min. The mass conditions were set as follows: ion source temperature, 200°C; scan range of 45 -600 m/z, and event time 0.5 s.
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10

Fatty Acid Profiling via GC-MS

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The extraction of lipids for fatty acids (FA) analysis was performed with chloroform/methanol (2:1 v/v), and FA methyl esters (FAME) were prepared according to Pérez-Palacios et al. [29 (link)] with some modifications. The FA composition of samples was identified using a gas chromatograph GC-2010 Plus (Shimadzu Europa GmbH, Duisburg, Germany) equipped with Mass Spectrometer GCMS-QP2010 (Shimadzu Europa GmbH, Duisburg, Germany). Separation was carried out on a Stabilwax-MS column (30 m length, 0.25 mmID, and 0.25 μm df) (Restek Corporation, Bellefonte, PA, USA). Oven temperature program started at 50 °C, then increased at a rate of 8 °C/min to 220 °C, held for 1 min at 220 °C, increased again at a rate of 20 °C/min to 240 °C and, finally, held throughout 10 min. The injector temperature was 240 °C, the interface −240 °C, and the ion source 240 °C. The carrier gas was helium at a flow rate of 0.91 mL/min. The individual FAME peaks were identified by comparing their retention times with FAME standards (Merck & Co., Inc., Kenilworth, NJ, USA).
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