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As 400 400 mhz spectrometer

Manufactured by Agilent Technologies

The AS-400 (400 MHz) spectrometer is a laboratory instrument designed for nuclear magnetic resonance (NMR) spectroscopy. It operates at a frequency of 400 MHz and is capable of analyzing the chemical composition and structure of various samples.

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2 protocols using as 400 400 mhz spectrometer

1

Synthesis and Characterization of Olaparib-BODIPY Conjugates

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Unless otherwise noted, all reagents were purchased from Sigma-Aldrich (St. Louis, MO) and used without further purification. BODIPY FL and BODIPY 650/665 succinimidyl ester were purchased from Invitrogen (Carlsbad, CA). Olaparib (AZD2281) was purchased from Selleck Chemicals (Houston, TX). 4-[[4-Fluoro-3-(piperazine-1-carbonyl)phenyl]methyl]-2H-phthalazin-1-one and olaparib-BODIPY FL were synthesized as described elsewhere (40 –42 (link)). HPLC-ESI-MS analyses and HPLC purifications were performed on a Waters (Milford, MA) LC-MS system. For LC-ESI-MS analyses, a Waters XTerra® C18 5 μm column was used. For preparative runs, an Atlantis® Prep T3 OBDTM 5 μM column was used. High-resolution ESI mass spectra were obtained on a Bruker Daltonics APEXIV 4.7 Tesla Fourier Transform mass spectrometer (FT-ICR-MS) in the Department of Chemistry Instrumentation Facility at the Massachusetts Institute of Technology. Proton nuclear magnetic resonance (1H NMR) spectra were recorded on a Varian AS-400 (400 MHz) spectrometer. Chemical shifts for protons are reported in parts per million (ppm) and are referenced against the dimethylsulfoxide lock signal (1H, 2.50 ppm). Data are reported as follows: chemical shift, multiplicity (s = singlet, d = doublet, t = triplet, m = multiplet), coupling constants (Hz) and integration.
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2

Analytical LC-MS and NMR Characterization

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Analytical LC-MS was performed on a
Waters 2545 HPLC equipped with a 2998 diode array detector, a Waters
3100 ESI-MS module, using a XTerraMS C18 5 μm, 4.6 × 50
mm column at a flow rate of 5 mL/min with a linear gradient (95% A:
5% B to 100% B with 90 and 30 s hold at 100% B, solvent A = water
+ 0.1% formic acid, solvent B = acetonitrile + 0.1% formic acid).
Proton and carbon nuclear magnetic resonance (1H and 13C NMR spectra) were recorded on a Varian AS-400 (400 MHz)
spectrometer. Chemical shifts for protons are reported in parts per
million (ppm) and are referenced to residual solvent peaks for C6H6 (7.16 ppm), CHCl3 (7.26 ppm), and
CH3CN (1.94 ppm). Data is reported as follows: chemical
shift, integration, multiplicity (s = singlet, d = doublet, t = triplet,
m = multiplet), and coupling constants (Hz). High-resolution mass-spectra
were performed on a Bruker Daltonics APEXIV 4.7 T Fourier transform
ion cyclotron resonance mass spectrometer (FT-ICR-MS), with ESI (Electro
Spray Ion) source. Instant JChem was used for structure database management,
search and prediction (Instant JChem 5.9.3, 2012, ChemAxon (http://www.chemaxon.com)).
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