Rapid, Quantitative Nuclear Magnetic Resonance Test for Oxygen-17 Enrichment in Water.

Autor: Peterson JW; Department of Chemistry and Biochemistry, Brigham Young University, Provo, Utah 84602, United States., Burt SR; Department of Chemistry and Biochemistry, Brigham Young University, Provo, Utah 84602, United States., Yuan Y; Department of Chemistry, University of Central Florida, 4111 Libra Drive, Orlando, Florida 32816, United States., Harper JK; Department of Chemistry and Biochemistry, Brigham Young University, Provo, Utah 84602, United States.
Jazyk: angličtina
Zdroj: Analytical chemistry [Anal Chem] 2022 Apr 19; Vol. 94 (15), pp. 5741-5743. Date of Electronic Publication: 2022 Apr 04.
DOI: 10.1021/acs.analchem.2c00081
Abstrakt: Nuclear magnetic resonance (NMR) studies involving 17 O are increasingly important in molecular biology, material science, and other disciplines. A large number of these studies employ H 2 17 O as a source of 17 O, and this reliance can be limiting because the high cost of H 2 17 O. To overcome this constraint, a recent study proposed a distillation scheme capable of producing significant quantities of H 2 17 O at a low cost. Although this method is reported to be effective, the reactions proposed to quantify percent of 17 O enrichment are either time intensive or have a risk of errors due to the isotope effect. Here, an alternative reaction scheme is described to measure 17 O water that ultimately creates methyl benzoate as the sole 17 O-containing product. The proposed reaction is completed in a matter of minutes at room temperature, produces only one 17 O product, and requires no clean-up step. The large isotope shift observed in solution NMR between the 13 C═ 16 O and 13 C═ 17 O resonances allows for integration of the individual peaks. This 13 C NMR analysis is found to be highly accurate over a wide enrichment range and is accessible to most NMR spectroscopists.
Databáze: MEDLINE