Application of Two-Dimensional ¹H−³¹P Inverse NMR Spectroscopy to the Detection of Trace Amounts of Organophosphorus Compounds Related to the Chemical Weapons Convention

Abstract

Two-dimensional (2D) 1 H-31 P NMR techniques are applied to samples containing trace amounts of organophosphorus (OP) compounds related to the Chemical Weapons Convention. Because these techniques allow the recording of 31 P-filtered spectra with the sensitivity of proton NMR, the problem of overlapping in 1 H NMR spectra is nearly canceled, while simultaneous 31 P and 1 H NMR information is obtained in a fast way. How these experiments are carried out is described. The advantages of 2D techniques are compared with respect to their 1D counterparts, and new developments are proposed for rapid and reliable assignment without the need for reference data of the spiked OP chemicals.

Use of NMR techniques for toxic organophosphorus compound profiling

“…sensitivity of proton and selectivity of phosphorus. An example of the application of 2D 1 H-31 P HSQC (heteronuclear single quantum coherence) [162] experiments in the OPCW Proficiency Test analysis was presented in 1997 by Albaret et al [163]. The soil sample that was analyzed in the test contained three OP compounds that were relevant to the CWC (Fig.…”

“…The proton resonances with JPH are shown in the spectrum, while the background resonances shown in the proton spectrum (top projection) are eliminated. The total acquisition time was 4 h 25 min.Reprinted with permission from[163]. Copyright 1997 American Chemical Society).…”

Simultaneous Determination of Theophylline and Caffeine by Proton Magnetic Resonance Spectroscopy Using Partial Least Squares Regression Techniques

“…The latter includes the determination of impurities, [14][15][16] the content of drugs [17][18][19] and the characterization of isomeric drug mixtures. 20,21 The complexity of the NMR spectra, which depends on overlapping signals, an interference problem or background noise, calls for the use of multivariate methods to resolve complex systems and to extract more information from a study of the generated data.…”

Complete 1H, 13C{1H}, and 31P NMR spectral parameters of some pyrophosphates

“…Several powerful NMR methods in determination of the structures of organophosphorus compounds have been published . In cases of decomposing compounds, the decomposition products can be used to identify the original chemicals.…”