Synthetic cathinones determination by liquid chromatography-mass spectrometry after ultrasound membrane assisted extraction

Autor: Cristian Suárez-Oubiña, Pamela Cabarcos-Fernández, Maria Jesús Tabernero-Duque, Pilar Bermejo-Barrera, Antonio Moreda-Piñeiro, Ana María Bermejo-Barrera
Přispěvatelé: Universidade de Santiago de Compostela. Departamento de Química Analítica, Nutrición e Bromatoloxía
Rok vydání: 2023
Předmět:
Zdroj: Microchemical Journal. 191:108869
ISSN: 0026-265X
Popis: The extraction time for membrane-assisted solvent extraction (MASE) when isolating synthetic cathinones from urine has been speeded up to 30 min by using ultrasounds. Separation and determination of eleven synthetic cathinones was further performed liquid chromatography-tandem mass spectrometry (LC-MS/MS). The ultrasound assisted MASE consisted of adjusting 5.0 mL of urine at pH 11.8 and performing the extractive process with 400 μL of n-hexane as an acceptor phase inside the polypropylene membrane under ultrasonication at room temperature. Synthetic cathinones exhibiting LogP values higher than 2.0, such as 3,4-dimethyl methcathinone, methylendioxypyrovalerone, and naphyrone), were efficiently extracted and pre-concentrated. Other synthetic cathinones (LogP between 2.0 and 0.7) were found to exhibit a lower mass transfer. The method was found to be matrix dependent, and a matrix-matched calibration was required for measurements. The achieved limits of detection (LOD) were between 0.03 (flephedrone) to 0.29 (ethylone) µg L-1, with relative standard deviations (RSDs) within the 6–14% and 7–19% ranges for intraday and inter-day assays, and intraday and inter-day analytical recoveries from 84 to 115% and 85 to 118%, respectively. The developed method was finally applied to urine samples from volunteers attending a music festival This work was supported by the Dirección Xeral de I + D – Xunta de Galicia Grupos de Referencia Competitiva (project number ED431C 2022/029) SI
Databáze: OpenAIRE