Diffusion-ordered spectroscopy on a benchtop spectrometer for drug analysis

Assemat, Gaëtan; Gouilleux, Boris; Bouillaud, Dylan; Farjon, Jonathan; Gilard, Véronique; Giraudeau, Patrick; Malet‐Martino, Myriam

doi:10.1016/j.jpba.2018.08.011

Cited by 31 publications

(41 citation statements)

References 32 publications

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“…A third pulse sequence adaptation recently made on a benchtop spectrometer is the DOSY experiment, which correlates chemical shifts and diffusion coefficients in two orthogonal dimensions, and is very popular for the analysis of mixtures at high field . This pulse sequence has been used in order to separate compounds from pharmaceutical formulation with a benchtop spectrometer . Although the conventional DOSY experiment is not compatible with online analysis, such limitation could be addressed in the future, thanks to the development of real‐time DOSY methods based on UF 2D NMR, which have already been applied at high‐field to dynamic chemical systems …”

Section: Applications Of Benchtop Nmr To the Study Of Bioprocessesmentioning

confidence: 99%

Benchtop NMR for the monitoring of bioprocesses

Bouillaud

Farjon

Gonçalves

et al. 2019

Magnetic Reson in Chemistry

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Benchtop NMR devices are transportable, convenient, and affordable, unlike high-field devices based on superconducting magnets. Such devices have opened numerous applications across a broad variety of scientific areas. This minireview focuses on the usefulness of benchtop nuclear magnetic resonance (NMR) for the monitoring of bioprocesses, highlighting new perspectives opened by the reduced size of devices in relaxometry, magnetic resonance imaging, and NMR spectroscopy. Using benchtop NMR in bioprocesses is not exempt of limitations-especially the loss of sensitivity and resolution arising from the use of a low magnetic field-and which are even further exacerbated by the sample complexity. Still, several studies have shown the efficiency of benchtop NMR in being a noninvasive probe to monitor the evolution of biological samples. If benchtop relaxometry and imaging have been developed for decades and have shown their capacity in monitoring such processes, the more recent emergence of the benchtop NMR spectroscopy gives a breath of fresh air for many applications and benefits from recent research led by spectroscopy specialists, which are adapted on these new devices, from nonconventional pulse sequences to advanced data processing. There is no doubt that these recent devices are powerful tools that will open numerous perspectives for the real-time study of bioprocesses in the coming years.

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Section: Applications Of Benchtop Nmr To the Study Of Bioprocessesmentioning

confidence: 99%

Benchtop NMR for the monitoring of bioprocesses

Bouillaud

Farjon

Gonçalves

et al. 2019

Magnetic Reson in Chemistry

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“…Low-field (LF) NMR is an emerging technique based on the use of a new generation of compact NMR [12][13][14]. A few applications of LF NMR in the pharmaceutical field have recently been described [15][16][17][18][19] and the feasibility of LF NMR for unveiling adulteration of DS has been demonstrated [15,19].…”

Section: Introductionmentioning

confidence: 99%

Chemometric Analysis of Low-field 1H NMR Spectra for Unveiling Adulteration of Slimming Dietary Supplements by Pharmaceutical Compounds

Balayssac

Danoun

et al. 2020

Molecules

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The recent introduction of compact or low-field (LF) NMR spectrometers that use permanent magnets, giving rise to proton (1H) NMR frequencies between 40 and 80 MHz, have opened up new areas of application. The two main limitations of the technique are its insensitivity and poor spectral resolution. However, this study demonstrates that the chemometric treatment of LF 1H NMR spectral data is suitable for unveiling medicines as adulterants of slimming dietary supplements (DS). To this aim, 66 DS were analyzed with LF 1H NMR after quick and easy sample preparation. A first PLS-DA model built with the LF 1H NMR spectra from forty DS belonging to two classes of weight-loss DS (non-adulterated, and sibutramine or phenolphthalein-adulterated) led to the classification of 13 newly purchased test samples as natural, adulterated or borderline. This classification was further refined when the model was made from the same 40 DS now considered as representing three classes of DS (non-adulterated, sibutramine-adulterated, and phenolphthalein-adulterated). The adulterant (sibutramine or phenolphthalein) was correctly predicted as confirmed by the examination of the 1H NMR spectra. A limitation of the chemometric approach is discussed with the example of two atypical weight-loss DS containing fluoxetine or raspberry ketone.

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“…[3] DOSY experiments were also reported and applied to the demixing of drugs formulations. [4] More recently, Pure-Shift (PS) methods [5] were implemented for the first time on a benchtop spectrometer, allowing significant line-narrowing in complex mixtures of small-to medium-sized molecules. [6] In addition to these advanced pulse-sequence developments, the study of reaction mixtures with possibly various mixed protonated solvents makes it crucial to selectively suppress multiple and intense undesired peaks from solvents or other compounds in order to detect the smallest ones coming from analytes of interest.…”

Section: Introductionmentioning

confidence: 99%

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

et al. 2020

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Emerging low cost, compact NMR spectrometers that can be connected in-line to a flow reactor are suited to study reaction mixtures. The main limitation of such spectrometers arises from their lower magnetic field inducing a reduced sensitivity and a weaker spectral resolution. For enhancing the spectral resolution, the merging of Pure-Shift methods recognized for line narrowing with solvent elimination schemes was implemented in the context of mixtures containing protonated solvents. One more step was achieved to further enhance the resolution power on compact systems, thanks to multiple elimination schemes prior to Pure-Shift pulse sequence elements. For the first time, we were able to remove up to 6 protonated solvent signals simultaneously by dividing their intensity by 500 to 1700 with a concomitant spectral resolution enhancement for signals of interest from 9 to 12 as compared to the standard 1D 1 H. Then, the potential of this new approach was shown on the flow synthesis of a complex benzoxanthenone structure.

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Diffusion-ordered spectroscopy on a benchtop spectrometer for drug analysis

Cited by 31 publications

References 32 publications

Benchtop NMR for the monitoring of bioprocesses

Benchtop NMR for the monitoring of bioprocesses

Chemometric Analysis of Low-field 1H NMR Spectra for Unveiling Adulteration of Slimming Dietary Supplements by Pharmaceutical Compounds

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

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