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Micromass lct mass spectrometer

Manufactured by Waters Corporation
Sourced in United States

The Micromass LCT® is a high-performance mass spectrometer designed for accurate mass measurement and analysis. It utilizes electrospray ionization (ESI) and time-of-flight (TOF) technology to provide precise mass determination of a wide range of molecules. The core function of the Micromass LCT® is to accurately measure the mass-to-charge ratio of ionized analytes, enabling the identification and characterization of various chemical compounds.

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6 protocols using micromass lct mass spectrometer

1

Synthesis and Characterization of ONB Ligands

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0.13 mmol of intermediate product II was dissolved in 2.3 mL of THF. In a separate container, 0.2 mmol of 3-aminopropane sulfonic acid sodium salt in 0.43 mL of water was added to the THF solution. The reaction was stirred overnight at 50 °C. The product was purified using a silica column with a mixture of dichloromethane:MeOH (1:5). The final product was confirmed by electrospray ionization mass spectrometry (ESI-MS). ESI mass spectra for the synthesized ligand molecules were obtained using a Waters (Micromass) LCT® mass spectrometer. ONB C12 (C24H38N3O8SNa), [M-Na+H+NH4]+: calculated m/z: 547.6, observed m/z: 547.3; ONB C8 (C20H30N3O8SNa), [M-Na+H+NH4]+: calculated m/z: 491.5, observed m/z: 491.3; ONB C6 (C18H26N3O8SNa), [M-Na+H+NH4]+: calculated m/z: 463.5, observed m/z: 463.3.
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2

PCNA Binding Kinetics of T2Pt

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Recombinant human PCNA (13.3 μM) was reacted with 0–50 μM T2Pt in 35 mM HEPES, pH 7.4, for 2 h at ambient temperature. Following the reaction, samples were filtered into 10 mM ammonium acetate by gel filtration (Micro Bio-Spin 6 chromatography column) to remove free T2Pt. Samples were subsequently desalted using a reverse phase c4 or c8 Zip Tip and eluted into 50% acetonitrile, 2% formic acid. The eluent was ionized by static nanospray using EconoTips on a Micromass LCT mass spectrometer [Waters (Milford, MA)] operating in positive mode. The resultant charge envelope was deconvoluted using MaxEnt 1 algorithm of MassLynx V 4.0 sp 4 software. A mass error of 1 Da for every 10,000 Da was permissible using this mass spectrometer.
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3

NMR and Spectroscopic Characterization of Novel Compounds

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1H (400 MHz), 13C{1H} (100 MHz), 31P{1H} (161 MHz) and 19F{1H} (376 MHz) NMR spectra were recorded on an Avance II+ 400 spectrometer (Bruker, Wissembourg, France) at 299 K (probe temperature). The chemical shifts are reported in parts per million (δ, ppm) and referenced to residual solvent peaks for 1H (CDCl3: δ = 7.26 ppm). The 31P- and 19F-NMR were referenced to the external aqueous solution of 85% H3PO4 and KF at 0.5 M, respectively in CDCl3 (or in a mixture of DMSO-D6/D2O for PPh3 spectra—see Supplementary Material, Figure S9). The IR spectra were measured on an Avatar 360 FTIR (Nicolet, Thermo Scientific, Waltham, MA, USA) in KBr pellets; only significant bands are mentioned in the text. The mass spectra (ESI-TOF) were recorded with a Micromass LCT mass spectrometer (Waters, Milford, MA, USA). Elemental analyses (C, H, N) were performed in a VariolEL instrument from Elementar Analysensysteme (Langenselbold, Germany). In the processing of the elemental analysis results of compound 3 and 4, the theoretical values were calculated taking into account the addition of dichloromethane molecules since their presence is observed in the 1H-NMR spectra of both compounds. This situation arises from the inclusion of solvent molecules and/or inorganic salts in the dendritic structures during the isolation of the compound by precipitation.
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4

Synthesis and Characterization of ONB Ligands

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0.13 mmol of intermediate product II was dissolved in 2.3 mL of THF. In a separate container, 0.2 mmol of 3-aminopropane sulfonic acid sodium salt in 0.43 mL of water was added to the THF solution. The reaction was stirred overnight at 50 °C. The product was purified using a silica column with a mixture of dichloromethane:MeOH (1:5). The final product was confirmed by electrospray ionization mass spectrometry (ESI-MS). ESI mass spectra for the synthesized ligand molecules were obtained using a Waters (Micromass) LCT® mass spectrometer. ONB C12 (C24H38N3O8SNa), [M-Na+H+NH4]+: calculated m/z: 547.6, observed m/z: 547.3; ONB C8 (C20H30N3O8SNa), [M-Na+H+NH4]+: calculated m/z: 491.5, observed m/z: 491.3; ONB C6 (C18H26N3O8SNa), [M-Na+H+NH4]+: calculated m/z: 463.5, observed m/z: 463.3.
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5

Native MS Analysis of Biomolecules

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Native MS was performed on a Micromass LCT mass spectrometer (Waters), calibrated using a 25 mg/ml CsI solution. Electrospray ionization was achieved from a gold-coated glass capillary, employing a capillary voltage of 1.2 kV, a sample cone voltage of 100 V, an extraction cone voltage of 10 V, a source temperature of 80 °C, and a source pressure of 8.8 mbar. Spectra were summed across 5 min, and smoothed for visualization purposes, whereas the m/z values were obtained from the centroids at 70% intensity.
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6

NMR, Mass Spectrometry, and DLS Analysis

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1H-NMR spectra were recorded on a Hermes-Varian Mercury Plus 300 (300 MHz) spectrometer at room temperature. Chemical shifts were recorded in parts per million (ppm) using residual solvent peaks as internal references [MeOH-d4 δ: 4.5 (1H) and DMSO-d6 δ: 2.5]. Electro spray ionization mass spectra for the synthesized ligand molecules were obtained using a Waters (Micromass) LCT® mass spectrometer (Waters, Beverly, MA) similarly as described previously.46 (link) High-resolution Fourier transformed ion cyclotron resonance (FT-ICR) mass spectra before and after UV irradiation were obtained on a 7 T LTQ/FT (Thermo Scientific, Waltham, MA), similarly as described in our previous publication.11 (link) DLS was carried out using a Malvern Zetasizer Nano. All DLS measurements of individual samples were performed three times after 120 sec equilibration.
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