Browsing by Author "Silva, Rodrigo Pelixo da"
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- Determination of ketamine and norketamine in hair samples by µ-QuEChERS and gas chromatography coupled to tandem mass spectrometryPublication . Silva, Rodrigo Pelixo da; Rosado, Tiago Alexandre Pires; Alba, Maria Eugénia Gallardo; Barroso, MárioKetamine (KET) has emerged as a popular new psychoactive substance in Europe due to the dissociative state it induces. These effects are sought by users at raves, as unprescribed remedies for psychological issues, and in drug-facilitated crimes. Forensic specialists often struggle to identify pathways to prove drug consumption; however, hair offers unparalleled advantages as a sample type that can reveal both chronic consumption and acute abuse, with cutting being the only way to prevent detection. As a complex matrix, hair requires pretreatment to remove interferences and enhance analysis sensitivity. This study employs a miniaturised version of the “Quick, Easy, Cheap, Rugged, and Safe” (QuEChERS) extraction method, commonly used in food and environmental analysis. The method involves the use of 1 mL of 5% formic acid (FA) in acetonitrile (ACN) and 250 mg NH4HCO2 as the solvent and salt partitioning agents, respectively, along with 50 mg of MgSO4 and 10 mg of PSA in the dispersive solid-phase extraction step. After this clean-up, the samples were analysed via gas chromatography coupled to tandem mass spectrometry. Following optimisation, the method was validated for the main drug and its primary metabolite, norketamine (NKET). A limit of detection (LOD) of 0.01 ng/mg was achieved for KET and 0.8 ng/mg for NKET, with a limit of quantification (LOQ) of 0.05 ng/mg and 0.8 ng/mg, respectively. Consequently, a working range of 0.05–5 ng/mg was established for KET, and 0.8–5 ng/mg for NKET. The recovery rates ranged from 47–76% for KET and 14–27% for NKET. Following this step, the method was applied to authentic samples collected from consumers. The µ-QuEChERS method proved to be a sustainable clean-up technique, maintaining the QuEChERS parameters despite its miniaturisation, and achieved high sensitivity, surpassing the cut-off value of 0.2 ng/mg established by the Society of Hair Testing.