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Maldi synapt g2 s hdms

Manufactured by Waters Corporation
Sourced in United States

The Maldi SYNAPT G2-S HDMS is a high-resolution mass spectrometry system designed for comprehensive biomolecular analysis. It features a MALDI (Matrix-Assisted Laser Desorption/Ionization) ion source and a SYNAPT G2-S HDMS (High-Definition Mass Spectrometry) analyzer. The system is capable of providing high-quality data for a range of applications, including protein characterization, small molecule identification, and structural elucidation.

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8 protocols using maldi synapt g2 s hdms

1

Synthesis and Antimicrobial Evaluation of Novel Compounds

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Starting materials and all other reagents were purchased from Sigma-Aldrich. All solvents were of analytical grade and were used without prior distillation. Merck silica gel plates 60 F254 were used for TLC (thin layer chromatography) analysis. Crude reaction mixtures were purified using column chromatography on Merck silica gel 60/230–400 mesh, with an appropriate mixture of hexane and ethyl acetate as a solvent. THF was dried according to standard procedure. Nuclear magnetic resonance spectra (NMR) were performed on a Bruker Avance 400 and Varian 500MHz instrument. Chemical shifts are expressed in ppm and coupling constant (J) in Hz using TMS as an internal standard. High-resolution mass spectra were acquired on a Maldi SYNAPT G2-S HDMS (Waters) apparatus with a QqTOF analyser.
The bacterial tests used, and MIC and MBC were accurately described in detail in the previous work [20 (link),21 (link),22 (link),23 (link),24 (link),25 (link),26 (link)]. An MTT test to assess the metabolic activity of cells was performed on the basis of [27 (link),28 ,29 (link),30 (link)], with THLE-5b as the control and the caco-2 cell line derived from human adenocarcinoma.
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2

NMR Spectroscopy of Organic Compounds

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All the chemicals were obtained from commercial sources and the solvents were of analytical grade. 1H and 13C NMR spectra were recorded in DMSO-d6, CDCl3 or acetone-d6 solution using Bruker Oxford 400 NMR spectrometer (400 MHz). Chemical shifts are expressed in parts per million using TMS as an internal standard. Low-resolution mass spectra were recorded on the API365i API 3000 spectrometer, and the ESI technique was used to analyte ionization. High-resolution mass spectra were recorded on the Maldi SYNAPT G2-S HDMS (Waters, Milford, MA, USA) apparatus with a QqTOF analyser.
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3

Organic Compound Synthesis and Purification

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Commercially available reagents were ordered from Sigma-Aldrich and used without additional purification. The water and hexanes mixtures were prior distilled. Other solvents (analytical grade) were used without extra drying and purification. Solvents and volatile reagents were evaporated under reduced pressure. Reactions were performed in dry glass vessel under ambient conditions. Merck silica gel plates 60 F254 were applied for TLC (Thin Layer Chromatography) analysis. Crude mixture, after solvent evaporation, were purified by column chromatography on Merck silica gel 60/230–400 mesh, using an appropriate mixture of hexane and ethyl acetate as solvent. 1H- and 13C NMR (Nuclear Magnetic Resonance) spectra were recorded in Chloroform-d at Bruker 400 and Varian 500 MHz sepctrometer using TMS (Trimethyl Silane) as an internal standard. Chemical shifts were reported in parts per million (ppm) and referred to residual deuterated solvent signal; coupling constants (J) were noted in Hz. High-resolution mass spectra (HR-MS) were recorded on the Maldi SYNAPT G2-S HDMS (Waters) apparatus with a QqTOF analyzer.
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4

Comprehensive Analytical Techniques for Materials Characterization

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NMR spectra were recorded on Bruker (400 MHz) instrument. GC–MS analyses were performed on PerkinElmer Clarus 680/600S. MS spectra were recorded on Maldi SYNAPT G2-S HDMS (Waters) spectrometer. UV–Vis spectra were recorded using Evolution220 spectrophotometer from Thermo Scientific. XPS spectra were recorded on PHI 5000 VersaProbe X-ray photoelectron spectrometer using an Al KR X-ray source. FT-IR spectra were recorded on Jasco 6200 instrument. SEM, STEM and EDX were recorded on FEI Nova NanoSEM 450.
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5

Comprehensive Chemical Characterization Methodology

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High-resolution mass spectra were obtained in the positive ion mode using Maldi-SYNAPT G2-S HDMS (Waters Corp., Milford, MA, USA) mass spectrometer equipped with an electrospray ion source and q-TOF type mass analyzer. 1H NMR spectra were recorded either in CDCl3 or in CD3OD on a Bruker AVANCE III HD 400 (resonance frequency 400.17 MHz) spectrometer (Bruker Corp., Billerica, MA, USA). Optical rotation was determined in CDCl3 on a PolAAr31 polarimeter (Optical Activity Ltd., Huntingdon, England). RP-HPLC separations were performed using an Agilent 1200 Series HPLC system (Agilent Technologies Inc., Santa Clara, CA, USA) equipped with a column oven and a diode array detector. Analytical chromatographic separations were carried out on a Kinetex XB-C18 column (4.6 × 250 mm, 5 μm total particle size; Phenomenex, Torrance, CA, USA). Semipreparative RP-HPLC was conducted on a Synergi 4μ Fusion-RP, 80A, 250 × 10 mm column (Phenomenex), with an isocratic elution, using MeOH–H2O mixtures of different polarities. Conventional column chromatography was carried out on Silica gel 60 (0.063–0.2 mm, Merck, Darmstadt, Germany). TLC separations were performed using precoated plates (Silica gel 60, Art. No 5553, Merck, Darmstadt, Germany).
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6

Synthesis and Analysis of Benzoamide Macrocycles

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The referenced
benzoamides (chemsets 3 and 4) were synthesized
as previously described, and the libraries were analyzed by HPLC on
a Bionacom Velocity C18-2 column (4.6 mm × 250 mm, grain size
5 μm) at 25 °C at a flow rate of 1 mL/min with gradient
elution (25% → 50% acetonitrile in water in 30 min).52 (link) To identify all of the macrocyclic hybrid tetraamides
(chemset 4hyb), the UPLC–MS
method was used (MALDI SYNAPT G2-S HDMS (Waters) connected with an
Acquity UPLC (Waters) at 25 °C at a flow rate of 1.5 mL/min with
gradient elution (25% → 50% acetonitrile in water in 30 min).
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7

UPLC-HRMS Analysis of Irradiated Samples

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Ultra performance liquid chromatography coupled to >high resolution mass spectrometry (UPLC-HRMS) analysis was performed using the ultra-performance liquid chromatograph ACQUITY UPLC I-Class (Waters Inc.) coupled with a MALDISynapt G2-S HDMS (Waters Inc.) mass spectrometer equipped with an electrospray ion source and quadrupole-time-of-flight mass analyzer. UPLC separations was done with the 2.1 × 100 mm ACQUITY UPLC BEH C18 (1.7 μm) column (Waters Inc.). Solvent A was water and solvent B was acetonitrile. The gradient flow was used from the 30% of solvent B as the initial conditions to the 100% of solvent B at 13 min, and it was maintained for 1 min and then back to initial conditions. The flow rate was 0.3 mL/min. The samples (ITR 0, 25 and 400 kGy) were diluted in acetonitrile. The peak at 2.40 min is present in all chromatograms and corresponds to the solvent background.
The measurements were performed in positive ion mode with the sampling cone set to 40 V and capillary voltage set to 3,000 V. The MSe experiments were set to collect the fragmentation spectra with the energy ramping from 30 to 50 eV.
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8

HPLC and MS Analysis of Lipids

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HPLC/UV and HPLC/MS analysis of lipids was performed as described earlier [27] . High resolution MS spectra were collected with the aid of MALDISynapt G2-S HDMS (Waters Inc) mass spectrometer equipped with an electrospray ion source and q-TOF type mass analyzer.
Tritiated lipids were analyzed with an on-line detector of radioactivity (Radiomatic, Packard, Canberra) coupled to the HPLC. Pren-28 was used as an internal standard.
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