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600 mhz nmr

Manufactured by Bruker
Sourced in Germany

The 600 MHz NMR is a nuclear magnetic resonance spectrometer that operates at a resonance frequency of 600 MHz for the 1H nucleus. It provides high-resolution analysis of molecular structures and compositions.

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10 protocols using 600 mhz nmr

1

NMR Spectroscopy for Styrene Incorporation

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1H NMR spectra were acquired in D2O using
a 600 MHz NMR (Bruker BioSpin, Rheinstetten, Germany) and processed
using TopSpin 4.0.9. The amount of incorporated styrene in P(AAm-co-St) was calculated as follows: where I7.3 ppm represents an integral of a triplet corresponding to protons of
phenyl groups (−C6H5) and I1.5–1.8 ppm an integral of protons corresponding
to methylene (−CH2−) groups present in the
polymer backbone.
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2

Dextran Reduction to Dextranol

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Dextran and the synthesized dextranol product were each dissolved in DMSO-d6 to approximate saturation. We spun tubes to remove the insoluble aggregates and added the supernatant (0.75 mL) to NMR tubes. We collected NMR spectra on Bruker 600 MHz NMR. Disappearance of anomeric proton peaks at 6.7 ppm and 6.3 ppm, corresponding to the alpha and beta stereoisomers of the anomeric center respectively, demonstrated the complete reduction to the alcohol [50 (link)].
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3

Cecal Metabolite Analysis by NMR

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Briefly, cecal contents were homogenized and filtered through a 3kDa membrane and metabolites extracted from the aqueous phase of water/chloroform/methanol mixture. Samples are analyzed on a Bruker 600MHz NMR containing 4,4-dimethyl-4-silapentane-1-sulfonic acid as internal standard.
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4

Large-Scale Enzymatic Product Analysis

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For the structure analysis of the enzymatic products, reactions were scaled-up to 10 mL containing FamD2 (5 μM), cyclase (20 μM), substrate (1 mM), GPP (1 mM), MgCl2 (5 mM), and CaCl2 (7.5 mM) in 50 mM Tris-HCl, pH 7.0 buffer. The reaction was incubated at 37 °C overnight, quenched and extracted with EtOAc, dried with Na2SO4 and concentrated. The extracted products were purified by HPLC. The purified compounds were concentrated, dissolved in C6D6, and analyzed using a Varian 600 MHz NMR and Bruker 800 MHz NMR.
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5

Quantitative NMR analysis of plasma acetate and TMA

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Quantitative measurements of acetate and TMA in plasma were determined by nuclear magnetic resonance spectroscopy (NMR). Briefly, plasma was filtered through a 3 kDa membrane filter (Merck Millipore) and polar metabolites extracted from the aqueous phase of a water:chloroform:methanol mixture. Samples, containing 4,4-dimethyl-4-silapentane-1-sulfonic acid as an internal standard, were analyzed on a Bruker 600 MHz NMR.
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6

NMR and LCMS Analysis of Compounds

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All compounds were procured through Sigma-Aldrich and Fisher Scientific. NMR spectra were collected using a Bruker 600 MHz NMR. LCMS data was collected using an Agilent 1290 Infinity Series LC system with 6150 MS. Column used was Agilent Eclipse Plus C18, 2.1 mm x 50 mm (8 μm). Mobile phase solvents were A: 0.05% formic acid; B: 5% water in acetonitrile. Runs consisted of 5% A for 0.5 minutes, gradient over 3 minutes of 5% A to 95% A, then 95% A over 1 minute. Synthesis of individual derivatives can be found in the Supporting Information.
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7

Structural Elucidation of Nesocodin by NMR

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First, 1 mg of the dried red solid nesocodin was dissolved in one mL of methanol-d4 containing 0.1% tetramethylsilane as an internal standard and transferred into a 5-mm thin-walled quartz NMR tube (Wilmad 535-PP-7). NMR data including one-dimensional (1D) 1H-NMR (SI Appendix, Fig. S11), two-dimensional 1H-double-quantum filtered correlation spectroscopy-NMR (2D 1H-DQF-COSY) (SI Appendix, Fig. S12), 1D 13C-NMR (with and without 1H decoupling) (SI Appendix, Fig. S13), two-dimensional heteronuclear single quantum coherence-NMR (2D HSQC-NMR) (SI Appendix, Fig. S13B), and two-dimensional Nuclear Overhauser Effect Spectroscopy-NMR (2D NOESY-NMR) (SI Appendix, Fig. S14) were obtained on a Bruker 600 MHz NMR at the University of Minnesota NMR Center on a fee-for-service basis and analyzed using TopSpin version 4.0.6.
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8

Characterization of Her-PEG-dMNPs

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The morphology of Her-PEG-dMNPs was characterized by using a JEM-2100F transmission electron microscope with an accelerating voltage of 200 kV, and the sample was made by using a film of copper mesh. Dynamic light scattering (DLS) was used to detect the hydrodynamic diameter of the dMNPs, PEG-dMNPs, and Her-PEG-dMNPs with a laser light-scattering spectrometer (SLS-5022F, Germany) 1H-NMR spectra of dMNPs and PEG-dMNPs were detected by a 600-MHz NMR (Bruker) spectrometer with D2O as the solvent.
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9

Purification and Characterization of Small Molecules

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Microwave reactions were carried out using a Biotage Initiator+ SP Wave microwave. Compounds were purified by preparative reverse phase HPLC using a Waters 1525 Binary HPLC pump equipped with a Waters 2487 dual absorbance detector system and a Waters Sunfire C18 OBD 5 μm 19 x 150 mm column. Absorbance was monitored at 345 and 220 nm. A gradient of 0-100% MeOH in H2O with 0.1% TFA over 60 min was used for compound purification. Purity was assessed by analytical HPLC using a Waters Symmetry C18 5 μm 4.6 x 150 mm column. Small molecules were analyzed using a gradient of 0-100% methanol in water with 0.1% TFA over 60 min. 1H NMR spectra were collected using a Bruker 400 MHz NMR, while 13C NMR spectra were collected on a Bruker 600 MHz NMR. High resolution mass spectrometry (HR-MS) was completed on an Applied Biosystems MALDI ToF Analyzer 4800 Plus using an α-cyano-4-hydroxycinnamic acid matrix with calibration standards. All compounds evaluated had ≥95% purity.
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10

Protein and Metabolite Profiling of IVD Tissue

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Fresh IVD tissue was ground and lysed in RIPA lysis buffer (Solarbio, Beijing, China) containing 1 mM phenylmethanesulfonyl fluoride (PMSF) and protease inhibitors to obtain protein. The concentration of the extracted protein was detected using a BCA kit (Solarbio, Beijing, China) according to the manufacturer's instructions. Five hundred microliter of D2O and 100 μl of 10% 3-(trimethylsilyl) propionic acid sodium salt (TSP) were then added to the protein. They were mixed and centrifuged at 14,000 g for 15 minutes (to remove the precipitated particles of the tissue in the solution). 550 μl of the supernatant was obtained and used to detect the protein and metabolite solution using the 600 MHz NMR (Bruker, Germany) equipment according to the manufacturer's instructions. The characteristic TOCSY, two-dimensional spectrum of the tissue metabolites and protein solution, was obtained and analyzed using the MestReNova (Mestrelab Research Co. Ltd., USA) software in order to identify the main differences in the metabolite and protein residues.
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