Quantitative NMR spectroscopy of complex mixtures

Giraudeau, Patrick

doi:10.1039/d3cc01455j

Cited by 10 publications

(15 citation statements)

References 148 publications

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“…Finally, the UF long-range HETCOR provides a peak-specific response factor, as any multi-pulse NMR experiment. With such peak-specific response, absolute quantification would require a calibration or standard additions procedures, as it is already the case for the vast majority of quantitative 2D NMR experiments 62 and as illustrated very recently in the case of hyperpolarised 1D 13 C NMR. Ribay et al showed that the absolute quantification of hyperpolarized natural abundance metabolites in freeze-dried urine samples was possible relying on a standard addition protocol, while retaining a repeatability of the concentration determination below 10%.…”

Section: Resultsmentioning

confidence: 99%

Optimization of heteronuclear ultrafast 2D NMR for the study of complex mixtures hyperpolarized by dynamic nuclear polarization

Praud,

Ribay,

Dey

et al. 2023

Anal. Methods

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Section: Resultsmentioning

confidence: 99%

Optimization of heteronuclear ultrafast 2D NMR for the study of complex mixtures hyperpolarized by dynamic nuclear polarization

Praud,

Ribay,

Dey

et al. 2023

Anal. Methods

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“…Besides solvent considerations, the choice of an instrumental detector is also important for obtaining informative chemical profiles of the global metabolome. NMR is indicated for many fingerprinting applications ,, and was used in this study. The main aim was to study if the significant effects determined by ASCA treating data separately for each individual solvent or mixture of the mixture design are retained on treating all of the mixture design data together in one data set.…”

Section: Introductionmentioning

confidence: 99%

¹H NMR Mixture Design–Fingerprints and ASCA Analysis in Ilex paraguariensis: Model Stability in Search of a Global Metabolome

Marcheafave,

Pauli,

Tormena

et al. 2023

Anal. Chem.

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The effects of experimental repetitions and solvent extractors on the 1H NMR fingerprinting of yerba mate extracts, obtained from two genders and two light environments, were analyzed in-depth by ANOVA–simultaneous component analysis (ASCA). Different solvents were used according to a mixture design based on ethanol, dichloromethane, and hexane and their combinations. The number of experimental repetitions significantly affected the ASCA results. Increasing repetitions led to decreases in the percentage effect variance values and an increase in the percentage residual variance. However, secondary sexual dimorphism, light availability, and their interaction effects became more significant with decreasing p-values at or above the 95% confidence level. The choice of a solvent extractor significantly affects the chemical profile and can lead to distinct conclusions regarding the significance of effect values. Pure solvents yielded different conclusions about the significance of factorial design effects, with each solvent extracting unique metabolites and maximizing information for specific effects. However, the use of binary solvent mixtures, such as ethanol–dichloromethane, proved more efficient in extracting sets of compounds that simultaneously differentiate between different experimental conditions. The mixture design–fingerprint strategy provided satisfactory results expanding the range of extracted metabolites with high percentage of residual variances and low explained percentage effect variances in the ASCA models. Ternary and even higher-ordered mixtures could be good alternative extracting media for work-intensive procedures. Our study underscores the significance of experimental design and solvent selection in metabolomic analysis, improving the accuracy, robustness, and interpretability of metabolomic models, leading to a better understanding of the chemical composition and biological implications of plant extracts.

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“…Determination of absolute concentrations can be performed by using internal or external reference standards or by synthetic signals with the desired peak attributes (i.e., ERETIC). 5 Another approach is to use the solvent peak or the peak of a known compound with a unique nonoverlapping signal. In both cases, the concentration should be readily and independently determined.…”

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confidence: 99%

Efficient Quantification of Milk Metabolites from ¹H NMR Spectra Using the Signature Mapping (SigMa) Approach: Chemical Shift Library Development for Cows’ Milk and Colostrum

Tsermoula,

Kristensen,

Mobaraki

et al. 2024

Anal. Chem.

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Cow milk contains essential nutrients for humans, and its bulk composition is usually analyzed using Fourier transform infrared spectroscopy. The higher sensitivity of nuclear magnetic resonance (NMR) spectroscopy can augment the extractible qualitative and quantitative information from milk to nearly 60 compounds, enabling us to monitor the health of cows and milk quality. Proton ( 1 H) NMR spectroscopy produces complex spectra that require expert knowledge for identifying and quantifying metabolites. Therefore, an efficient and reproducible methodology is required to transform complex milk 1 H NMR spectra into annotated and quantified milk metabolome data. In this study, standard operating procedures for screening the milk metabolome using 1 H NMR spectra are developed. A chemical shift library of 63 milk metabolites was established and implemented in the open-access Signature Mapping (SigMa) software. SigMa is a spectral analysis tool that transforms 1 H NMR spectra into a quantitative metabolite table. The applicability of the proposed methodology to whole milk, skim milk, and ultrafiltered milk is demonstrated, and the method is tested on ultrafiltered colostrum samples from dairy cows (n = 88) to evaluate whether metabolic changes in colostrum may reflect the metabolic status of cows.

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Quantitative NMR spectroscopy of complex mixtures

Abstract: Complex mixtures are ubiquitous in many branches of chemistry, be it a complex pharmaceutical formulation, a collection of biofluids analysed in a metabolomics workflow, or a flowing mixture in a...

Cited by 10 publications

References 148 publications

Optimization of heteronuclear ultrafast 2D NMR for the study of complex mixtures hyperpolarized by dynamic nuclear polarization

Optimization of heteronuclear ultrafast 2D NMR for the study of complex mixtures hyperpolarized by dynamic nuclear polarization

¹H NMR Mixture Design–Fingerprints and ASCA Analysis in Ilex paraguariensis: Model Stability in Search of a Global Metabolome

Efficient Quantification of Milk Metabolites from ¹H NMR Spectra Using the Signature Mapping (SigMa) Approach: Chemical Shift Library Development for Cows’ Milk and Colostrum

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Quantitative NMR spectroscopy of complex mixtures

Abstract: Complex mixtures are ubiquitous in many branches of chemistry, be it a complex pharmaceutical formulation, a collection of biofluids analysed in a metabolomics workflow, or a flowing mixture in a...

Cited by 10 publications

References 148 publications

Optimization of heteronuclear ultrafast 2D NMR for the study of complex mixtures hyperpolarized by dynamic nuclear polarization

Optimization of heteronuclear ultrafast 2D NMR for the study of complex mixtures hyperpolarized by dynamic nuclear polarization

1H NMR Mixture Design–Fingerprints and ASCA Analysis in Ilex paraguariensis: Model Stability in Search of a Global Metabolome

Efficient Quantification of Milk Metabolites from 1H NMR Spectra Using the Signature Mapping (SigMa) Approach: Chemical Shift Library Development for Cows’ Milk and Colostrum

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Product

Resources

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¹H NMR Mixture Design–Fingerprints and ASCA Analysis in Ilex paraguariensis: Model Stability in Search of a Global Metabolome

Efficient Quantification of Milk Metabolites from ¹H NMR Spectra Using the Signature Mapping (SigMa) Approach: Chemical Shift Library Development for Cows’ Milk and Colostrum