Merging Gradient‐Based Methods to Improve Benchtop NMR Spectroscopy: A New Tool for Flow Reaction Optimization

Kunjir, Shrikant; Rodriguez‐Zubiri, Mireia; Coeffard, Vincent; Felpin, François‐Xavier; Giraudeau, Patrick; Farjon, Jonathan

doi:10.1002/cphc.202000573

Cited by 5 publications

(8 citation statements)

References 18 publications

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“…In this regard, Morris et al have shown that PSYCHE with water suppression using excitation sculpting (ES) can be successfully applied to record 1 H pure shift spectra of ubiquitin in 90% H 2 O/10% D 2 O . Farjon et al have also combined pure shift methods and WET180 presaturation technique using a benchtop low-field NMR spectrometer to analyze simple mixtures of metabolites . To date, the problem of suppressing the water signal from pure shift spectra recorded for the purpose of metabolic profiling on a high-resolution NMR spectrometer has not been tackled yet.…”

Section: Introductionmentioning

confidence: 99%

Ultrahigh-Resolution NMR with Water Signal Suppression for a Deeper Understanding of the Action of Antimetabolic Drugs on Diffuse Large B-Cell Lymphoma

et al. 2022

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Ultrahigh-resolution NMR has recently attracted considerable attention in the field of complex samples analysis. Indeed, the implementation of broadband homonuclear decoupling techniques has allowed us to greatly simplify crowded 1 H spectra, yielding singlets for almost every proton site from the analyzed molecules. Pure shift methods have notably shown to be particularly suitable for deciphering mixtures of metabolites in biological samples. Here, we have successfully implemented a new pure shift pulse sequence based on the PSYCHE method, which incorporates a block for solvent suppression that is suitable for metabolomics analysis. The resulting experiment allows us to record ultrahigh-resolution 1D NOESY 1 H spectra of biofluids with suppression of the water signal, which is a crucial step for highlighting metabolite mixtures in an aqueous phase. We have successfully recorded pure shift spectra on extracellular media of diffuse large B-cell lymphoma (DLBCL) cells. Despite a lower sensitivity, the resolution of pure shift data was found to be better than that of the standard approach, which provides a more detailed vision of the exo-metabolome. The statistical analyses carried out on the resulting metabolic profiles allow us to successfully highlight several metabolic pathways affected by these drugs. Notably, we show that Kidrolase plays a major role in the metabolic pathways of this DLBCL cell line.

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Section: Introductionmentioning

confidence: 99%

Ultrahigh-Resolution NMR with Water Signal Suppression for a Deeper Understanding of the Action of Antimetabolic Drugs on Diffuse Large B-Cell Lymphoma

et al. 2022

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“… 112 The variety of nuclei, techniques, and ongoing advances also makes this method widely applicable to different chemistries, which may not be suitable for MS or chromatography. 113 For example, insights gained from mechanistic analysis can inform reaction optimization and flow NMR has been utilized for the in situ study of reactive organometallics representing catalytic intermediates. 114 Even common challenges in NMR such as overlapping peaks have been overcome utilizing state of the art algorithms.…”

Section: Data Collectionmentioning

confidence: 99%

“…Flow NMR has the advantage of having highly transferable data analysis, high information content, and moderate acquisition times (∼0.5 s scan –1 ) . The variety of nuclei, techniques, and ongoing advances also makes this method widely applicable to different chemistries, which may not be suitable for MS or chromatography . For example, insights gained from mechanistic analysis can inform reaction optimization and flow NMR has been utilized for the in situ study of reactive organometallics representing catalytic intermediates .…”

Section: Data Collectionmentioning

confidence: 99%

Chemputation and the Standardization of Chemical Informatics

Hammer

Leonov

Bell

et al. 2021

JACS Au

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The explosion in the use of machine learning for automated chemical reaction optimization is gathering pace. However, the lack of a standard architecture that connects the concept of chemical transformations universally to software and hardware provides a barrier to using the results of these optimizations and could cause the loss of relevant data and prevent reactions from being reproducible or unexpected findings verifiable or explainable. In this Perspective, we describe how the development of the field of digital chemistry or chemputation, that is the universal code-enabled control of chemical reactions using a standard language and ontology, will remove these barriers allowing users to focus on the chemistry and plug in algorithms according to the problem space to be explored or unit function to be optimized. We describe a standard hardware (the chemical processing programming architecture—the ChemPU) to encompass all chemical synthesis, an approach which unifies all chemistry automation strategies, from solid-phase peptide synthesis, to HTE flow chemistry platforms, while at the same time establishing a publication standard so that researchers can exchange chemical code (χDL) to ensure reproducibility and interoperability. Not only can a vast range of different chemistries be plugged into the hardware, but the ever-expanding developments in software and algorithms can also be accommodated. These technologies, when combined will allow chemistry, or chemputation, to follow computation—that is the running of code across many different types of capable hardware to get the same result every time with a low error rate.

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“…Their lower sensitivity can sometimes be offset by concentrating the samples or using a variety of methodologies for the enhancement of Boltzmann polarization [ 4 ]. Similarly, issues with chemical shift resolution can be addressed through the application of different signal acquisition and processing techniques, including solvent suppression and gradient-based pulse sequences [ 3 , 5 ].…”

Section: Introductionmentioning

confidence: 99%

Predicting Mandarin Fruit Acceptability: From High-Field to Benchtop NMR Spectroscopy

Migues

Rivas

Moyna

et al. 2022

Foods

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Recent advances in nuclear magnetic resonance (NMR) have led to the development of low-field benchtop NMR systems with improved sensitivity and resolution suitable for use in research and quality-control laboratories. Compared to their high-resolution counterparts, their lower purchase and running costs make them a good alternative for routine use. In this article, we show the adaptation of a method for predicting the consumer acceptability of mandarins, originally reported using a high-field 400 MHz NMR spectrometer, to benchtop 60 MHz NMR systems. Our findings reveal that both instruments yield comparable results regarding sugar and citric acid levels, leading to the development of virtually identical predictive linear models. However, the lower cost of benchtop NMR systems would allow cultivators to implement this chemometric-based method as an additional tool for the selection of new cultivars.

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Merging Gradient‐Based Methods to Improve Benchtop NMR Spectroscopy: A New Tool for Flow Reaction Optimization

Cited by 5 publications

References 18 publications

Ultrahigh-Resolution NMR with Water Signal Suppression for a Deeper Understanding of the Action of Antimetabolic Drugs on Diffuse Large B-Cell Lymphoma

Ultrahigh-Resolution NMR with Water Signal Suppression for a Deeper Understanding of the Action of Antimetabolic Drugs on Diffuse Large B-Cell Lymphoma

Chemputation and the Standardization of Chemical Informatics

Predicting Mandarin Fruit Acceptability: From High-Field to Benchtop NMR Spectroscopy

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