Salicylate poisoning detected by 1H NMR spectroscopy.

NMR spectroscopy reveals acetylsalicylic acid metabolites in the human urine for drug compliance monitoring

“…The study of urine samples of volunteers before and after oral administration of 100, 300, and 3000 mg of aspirin revealed significant changes in one and two-dimensional 1 H NMR spectra associated with the presence of additional signals attributed to salicyluric acid. A review of the literature reveals the variability of data on the content of the major metabolites of ASA in urine after taking aspirin [18][19][20]. The relative concentration depends on the dose taken by subjects and on the kinetics of excretion of metabolites.…”

“…All spectra were acquired at 25° C. The assignment of signals is given relative to TMS. Spectral assignment of endogenous compounds in urine samples was performed by taking into account the literature data on chemical shifts in biological fluids and spin-spin interaction constants [ 17 , 18 ]. Preliminarily, in order to distinguish the signals of aspirin metabolites against the background of healthy human metabolites, such as hippuric acid, 1 H NMR spectra of standard compounds, purchased from Sigma-Aldrich (salicylic, salicyluric and gentisic acids, corresponding to the major metabolites of acetylsalicylic acid and hippuric acid) were recorded under the same experimental conditions as urine samples.…”

“…The NMR method has been successfully used to detect metabolites in urine and blood in the case of salicylate poisoning and drug overdose [18][19][20]. However, there is no research focused on ASA analysis of metabolites related to patient compliance monitoring.…”

“…NMR spectroscopy is recognized as a rapid, non-invasive, reliable method for metabolomic studies in biological fluids, such as urine or blood, and used in order to develop new analytical methods for diagnosing diseases [ 17 , 18 ]. The main advantages of NMR are the non-destructive nature of NMR spectroscopy and the relative simplicity of sample preparation, as the latter does not require chromatographic separation or chemical derivatization, and high level of experimental reproducibility.…”

“…The advantage of the NMR method over LC-MS is the possibility to quantify more than 200 components of various chemical nature within a single experiment in a relatively short time, within minutes or seconds after the spectra have been collected [ 18 , 19 ].…”