A precise and rapid isotopomic analysis of small quantities of cholesterol at natural abundance by optimized 1H-13C 2D NMR - Archive ouverte HAL Accéder directement au contenu
Article Dans Une Revue Analytical and Bioanalytical Chemistry Année : 2021

A precise and rapid isotopomic analysis of small quantities of cholesterol at natural abundance by optimized 1H-13C 2D NMR

Résumé

Cholesterol, the principal zoosterol, is a key metabolite linked to several health complications. Studies have shown its potential as a metabolic biomarker for predicting various diseases and determining food origin. However, the existing INEPT (insensitive nuclei enhanced by polarization transfer) 13C position-specific isotope analysis method of cholesterol by NMR was not suitable for very precise analysis of small quantities due to its long acquisition time and therefore is restricted to products rich in cholesterol. In this work, a symmetric and adiabatic heteronuclear single quantum coherence (HSQC) 2D NMR sequence was developed for the high-precision (few permil) analysis of small quantities of cholesterol. Adiabatic pulses were incremented for improving precision and sensitivity. Moreover, several strategies such as the use of non-uniform sampling, linear prediction, and variable recycling time were optimized to reduce the acquisition time. The number of increments and spectral range were also adjusted. The method was developed on a system with a cryogenically cooled probe and was not tested on a room-temperature system. Our new approach allowed analyzing as low as 5 mg of cholesterol in 31 min with a long-term repeatability lower than 2‰ on the 24 non-quaternary carbon atoms of the molecule comparing to 16.2 h for the same quantity using the existing INEPT method. This result makes conceivable the isotope analysis of matrices low in cholesterol. Graphical abstract
Fichier non déposé

Dates et versions

hal-03376112 , version 1 (13-10-2021)

Identifiants

Citer

Lenny Haddad, Sophie Renou, Gérald Remaud, Toufic Rizk, Joseph Bejjani, et al.. A precise and rapid isotopomic analysis of small quantities of cholesterol at natural abundance by optimized 1H-13C 2D NMR. Analytical and Bioanalytical Chemistry, 2021, 413 (6), pp.1521-1532. ⟨10.1007/s00216-020-03135-0⟩. ⟨hal-03376112⟩
44 Consultations
0 Téléchargements

Altmetric

Partager

Gmail Facebook X LinkedIn More