Analysis of new psychoactive substances in human urine by ultra‐high performance supercritical fluid and liquid chromatography: Validation and comparison

Abstract

New psychoactive substances represent serious social and health problem as tens of new compounds are detected in Europe annually. They often show structural proximity or even isomerism, which complicates their analysis. Two methods based on ultra high performance supercritical fluid chromatography and ultra high performance liquid chromatography with mass spectrometric detection were validated and compared. A simple dilute-filter-and-shoot protocol utilizing propan-2-ol or methanol for supercritical fluid or liquid chromatography, respectively, was proposed to detect and quantify 15 cathinones and phenethylamines in human urine. Both methods offered fast separation (<3 min) and short total analysis time. Precision was well <15% with a few exceptions in liquid chromatography. Limits of detection in urine ranged from 0.01 to 2.3 ng/mL, except for cathinone (5 ng/mL) in supercritical fluid chromatography. Nevertheless, this technique distinguished all analytes including four pairs of isomers, while liquid chromatography was unable to resolve fluoromethcathinone regioisomers. Concerning matrix effects and recoveries, supercritical fluid chromatography produced more uniform results for different compounds and at different concentration levels. This work demonstrates the performance and reliability of supercritical fluid chromatography and corroborates its applicability as an alternative tool for analysis of new psychoactive substances in biological matrixes.

Ultra‐high performance supercritical fluid chromatography combined with quadrupole time‐of‐flight mass spectrometry for the characterization of pentaerythritol fatty acid esters

“…In addition, UHPSFC is a green technology (or clean technology), with shorter analysis time, less use of organic solvents, and wider range of applications. 6,7 UHPSFC for the analysis of pentaerythritol fatty acid esters has the merits of short analysis time and high separation efficiency, owing to the properties of the supercritical fluid. To the best of our knowledge, no paper has been published on the separation of pentaerythritol fatty acid esters using UHPSFC.…”

“…Accordingly, SFC facilitates high‐throughput and high‐resolution analysis. In addition, UHPSFC is a green technology (or clean technology), with shorter analysis time, less use of organic solvents, and wider range of applications . UHPSFC for the analysis of pentaerythritol fatty acid esters has the merits of short analysis time and high separation efficiency, owing to the properties of the supercritical fluid.…”

Supercritical fluid chromatography – Mass spectrometry: Recent evolution and current trends

“…This aspect is being currently investigated by several authors, with a growing number of publications [38,39,45,47,49,75] showing that the validation procedure in SFC-MS yields similar, if not even better results than LC-MS. Indeed, during different validation processes of SFC-MS methods, it was found that SFC-MS manages to provide better results in terms of identification, reproducibility, precision and accuracy when compared to LC-MS [47,75]. These findings are extremely important in establishing SFC-MS itself as a technique that is compatible with regulated bioanalytical laboratories.…”

Cyclic Ion Mobility of Isomeric New Psychoactive Substances Employing Characteristic Arrival Time Distribution Profiles and Adduct Separation

“…A fast chromatographic run (1.6 min) was sufficient to analyze a mixture of 15 NPS and separate isomers . For the detection and quantification of NPS in urine samples, the SFC-MS method was competitive with LC-MS …”