NMR reaction monitoring in flow synthesis

Gómez, M. Victoria; Hoz, Antonio de la

doi:10.3762/bjoc.13.31

Cited by 76 publications

(54 citation statements)

References 46 publications

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“…Hyperpolarisation (HP) of nuclear spins greatly enhances signal 13 intensities, with the potential to significantly expand the scope of both spectroscopic NMR and MRI 14 systems, as well as sensing technologies [20]. The most well-known derivative of this technique, 15 dynamic nuclear polarisation (DNP), engenders several hundred-fold increases in sensitivity for solid 16 material analytes [21]. Moreover, in solution, DNP has been shown to increase sensitivity up to ten 17 thousand times under standard conditions, opening up a variety of applications for lower frequency 18 spectrometers [19].…”

Section: Experimental Developments 1mentioning

confidence: 99%

Progress in Low Field Benchtop NMR Spectroscopy in Chemical and Biochemical Analysis

Grootveld¹,

Percival²,

Gibson³

et al. 2019

Preprint

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Section: Experimental Developments 1mentioning

confidence: 99%

Progress in Low Field Benchtop NMR Spectroscopy in Chemical and Biochemical Analysis

Grootveld¹,

Percival²,

Gibson³

et al. 2019

Preprint

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show abstract

“…On‐line reaction monitoring requires new pulse sequences (NOESY with WET sequence to suppress the protonated solvent signal). Bubbles and turbulent flow regimes distort NMR signals . A single scan acquisition in a 60 MHz bench top spectrometer produces quantitative kinetic data for small molecules at a concentration of 1 mmol

\cdot

L −1 , flowing in a PTFE tube at 1 mL

\cdot

min −1 .…”

Section: Uncertaintymentioning

confidence: 99%

Experimental Methods in Chemical Engineering: Nuclear Magnetic Resonance

2019

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Nuclear magnetic resonance (NMR) spectroscopy measures free induction decay (FID) signals that atomic nuclei emit when excited by a radiofrequency (RF) pulse in a static magnetic field. The Fourier-transformed spectrum shows chemically shifted peaks, area intensity, and multiplicity, which give information on molecular structure, bonds, functional groups, and purity. Web of Science Core Collection indexed 46 000 articles that mentioned NMR in 2016 and 2017. The VosViewer software grouped the research into 5 clusters: solid-state analysis including metabolomics; biology with in-vitro and antibacterial applications; coupled analytical techniques to identify crystal structure for which x-ray diffraction and density functional theory figure prominently; liquid-state analysis for polymers, aqueous solutions, nano-particles, and drug delivery; and chemosensors. Researchers publishing in The Canadian Journal of Chemical Engineering focus most on: liquid-state NMR to characterize polymers, branching, and monomers; quantify conformation, reaction kinetics, and equilibrium; and assess surfactant stability, ionic liquids, and composition. We introduce the theory behind NMR spectroscopy and common applications in chemistry and material science. We highlight the strength and limitations, sources of error, and the detection limit for this analytical technique, as manufacturers develop massive magnets for high-resolution spectra (1 GHz), and benchtop NMR for real-time, in-situ analysis (80 MHz).

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“…Therefore, high-resolution spectra are achievable of molecules being consumed by, and excreted from, the biological sample in the bioreactor. This approach has been successfully implemented to monitor chemical reactions [ 24 , 25 , 26 , 27 , 28 , 29 , 30 ], including the use of low-field benchtop NMR spectrometers for both chemical [ 31 , 32 ] and biological applications [ 33 , 34 ]. Importantly, the interface to the NMR spectrometer is simplified in comparison with the in situ operation mode: only tubing and pumps are required for sample shuttling from a suitable external bioreactor station; in effect, the biological culturing becomes a module to be coupled to the NMR measurement system.…”

Section: Introductionmentioning

confidence: 99%

A Nuclear Magnetic Resonance (NMR) Platform for Real-Time Metabolic Monitoring of Bioprocesses

et al. 2020

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We present a Nuclear Magnetic Resonance (NMR) compatible platform for the automated real-time monitoring of biochemical reactions using a flow shuttling configuration. This platform requires a working sample volume of ∼11 mL and it can circulate samples with a flow rate of 28 mL/min., which makes it suitable to be used for real-time monitoring of biochemical reactions. Another advantage of the proposed low-cost platform is the high spectral resolution. As a proof of concept, we acquire 1H NMR spectra of waste orange peel, bioprocessed using Trichoderma reesei fungus, and demonstrate the real-time measurement capability of the platform. The measurement is performed over more than 60 h, with a spectrum acquired every 7 min, such that over 510 data points are collected without user intervention. The designed system offers high resolution, automation, low user intervention, and, therefore, time-efficient measurement per sample.

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NMR reaction monitoring in flow synthesis

Cited by 76 publications

References 46 publications

Progress in Low Field Benchtop NMR Spectroscopy in Chemical and Biochemical Analysis

Progress in Low Field Benchtop NMR Spectroscopy in Chemical and Biochemical Analysis

Experimental Methods in Chemical Engineering: Nuclear Magnetic Resonance

A Nuclear Magnetic Resonance (NMR) Platform for Real-Time Metabolic Monitoring of Bioprocesses

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