Abstract

In this paper, a natural deep eutectic solvent (NADES)-based liquid phase microextraction (LPME) of 20 pharmaceuticals from urine, employing liquid chromatography tandem mass spectrometry (LC-MS/MS) for precise quantification, has been developed. The chromatographic gradient was accurately evaluated to ensure the effective separation of tramadol, an opioid receptor agonist, and o-desmethylvenlafaxine, one active metabolite of the antidepressant venlafaxine, both compounds sharing identical molecular mass for the precursor ion (Q1: 264.2 m/z) and fragmentation patterns (Quantifier ion: 58.2 m/z; qualifier ion: 246.0 m/z). NADES consisted of menthol-octanoic acid in a molar ratio of 1:2. Using the appropriate extraction conditions, the developed methodology provided appropriate LOQ values, ranging from 15 to 208 ng L–1, with reasonable RSD values (below 11 %), recoveries ranging from 64 to 120 % and preconcentration factors up to 66.6 folds. Application of the developed method to the analysis of urine samples served to highlight its usefulness. An AGREEprep score of 0.64 was obtained despite the demand for substantial sample volumes and the use of LC-MS/MS for analyte determination.

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