Determination of isotope abundance for deuterium‐labeled compounds by quantitative ¹H NMR + ²H NMR

Abstract

Deuterated reagents have been used in many research fields. Isotope abundance, as the feature parameter of deuterated reagents, the precise quantification, is of great importance. Based on quantitative nuclear magnetic resonance technology, a novel method that combines 1H NMR + 2H NMR was systematically established to determine the isotopic abundance of deuterated reagents. The results showed that the isotopic abundance of partially labeled and fully labeled compounds calculated by this new method was even more accurate than that calculated by classical 1H NMR and mass spectrometry (MS) methods. In brief, this new method is a robust strategy for the determination of isotope abundance in large‐scale deuterated reagents.

Rapid characterization of isotopic purity of deuterium‐labeled organic compounds and monitoring of hydrogen–deuterium exchange reaction using electrospray ionization‐high‐resolution mass spectrometry

“…Currently, the research strategies of isotopic purity of stable isotopes mainly contain a series of methods based on mass spectrometry (MS), [13][14][15][16] infrared spectroscopy (IR), 17,18 Raman spectroscopy, 19 and quantitative nuclear magnetic resonance (qNMR). [20][21][22][23][24] Precise quantification of isotopic purity is imperative for scientific research and the quality control of deuterium-labeled reagents. Therefore, the development of characterization and calculation methods for analyzing isotopic purity is of great significance.…”

“…Therefore, the development of characterization and calculation methods for analyzing isotopic purity is of great significance. 23 However, compared with NMR methods, high-resolution mass spectrometry (HRMS) does not need prior knowledge of specific spectra and information on chemical shifts. NMR method is not suitable for all deuterium-labeled organic compounds, especially when compounds easily tautomerize on the deuterium labeling positions to isomers.…”

“…Precise quantification of isotopic purity is imperative for scientific research and the quality control of deuterium‐labeled reagents. Therefore, the development of characterization and calculation methods for analyzing isotopic purity is of great significance 23 . However, compared with NMR methods, high‐resolution mass spectrometry (HRMS) does not need prior knowledge of specific spectra and information on chemical shifts.…”

“…With the rapid development of analytical instruments and increasing requirements under new trends, the use of isotopic purity characterization methods has substantially increased. Currently, the research strategies of isotopic purity of stable isotopes mainly contain a series of methods based on mass spectrometry (MS), 13–16 infrared spectroscopy (IR), 17,18 Raman spectroscopy, 19 and quantitative nuclear magnetic resonance (qNMR) 20–24 . Precise quantification of isotopic purity is imperative for scientific research and the quality control of deuterium‐labeled reagents.…”