An Easy and Reliable Method for the Mitigation of Deuterated Chloroform Decomposition to Stabilise Susceptible NMR Samples

Highly reactive decomposition products of deuterated chloroform can deteriorate samples dissolved in this commonly used solvent for nuclear magnetic resonance (NMR) spectroscopy. Samples for metabolomics studies often contain a complex mixture of sensitive substances such as phospholipids, peptides,...

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Bibliographic Details
Published in:Chemistry an international journal 2022-08, Vol.4 (3), p.776-785
Main Authors: Teipel, Jan, Gottstein, Vera, Hölzle, Eva, Kaltenbach, Katja, Lachenmeier, Dirk, Kuballa, Thomas
Format: Article
Language:English
Subjects:
Carbon dioxide
chemometrics
Chlorine
Chloroform
Coffee
Decomposition reactions
Deuteration
Eggs
Fatty acids
Hydrochloric acid
Metabolites
metabolomics
multivariate data evaluation
NMR
NMR spectroscopy
non-targeted analysis
Nuclear magnetic resonance
Peptides
Phosgene
Phospholipids
Reaction products
Reproducibility
Spectra
Spectrum analysis
Vitamins
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Summary:Highly reactive decomposition products of deuterated chloroform can deteriorate samples dissolved in this commonly used solvent for nuclear magnetic resonance (NMR) spectroscopy. Samples for metabolomics studies often contain a complex mixture of sensitive substances such as phospholipids, peptides, unsaturated fatty acids or vitamins. If these react with decomposition products (of chloroform), abnormal NMR spectra could result, e.g., signal shifts depending on pH, attenuation of signals over time due to chemical changes of analytes or new signals from reaction products. Such irreproducibly influenced spectra are especially problematic for non-targeted analysis methods using automated chemometrical data evaluation. To prevent these artefacts, chlorine, phosgene and hydrochloric acid need to be eliminated from deuterated chloroform before its use. Since the common stabilisation methods have proven to be insufficient for sensitive NMR samples, another purging method has been tested: Mitigation is easily and reliably achieved by washing the deuterated chloroform with concentrated disodium carbonate solution and subsequent desiccation with oven-dried disodium carbonate.
ISSN:2624-8549
2624-8549
DOI:10.3390/chemistry4030055