RT Journal Article
T1 Ultrasound assisted membrane-assisted solvent extraction for the simultaneous assessment of some drugs involved in drug-facilitated sexual assaults by liquid chromatography-tandem mass spectrometry
A1 Justo Vega, Ana
A1 Jinadasa, Kamal K.
A1 Jayasinghe, Gabadage Dona Thilini Madurangika
A1 Álvarez Freire, Iván
A1 Bermejo Barrera, Ana María
A1 Bermejo Barrera, Pilar
A1 Moreda Piñeiro, Antonio
K1 Drug-facilitated sexual assault
K1 Urine
K1 Membrane assisted solvent extractio
AB A simple and highly efficient ultrasound assisted membrane-assisted solvent extraction (MASE) pre-treatment method for urine has been developed and validated for the simultaneous determination of twenty-two drugs involved in drug-facilitated sexual assaults (DFSAs) by liquid chromatography-tandem mass spectrometry. MASE was performed with 4.0 mL of urine (pH adjusted at 12), 400 μL of hexane as an organic solvent inside the polypropylene membrane, and ultrasonication (45 kHz, 120 W) for 10 min. A pre-concentration factor of 40 was achieved after evaporation (N2 stream) and re-dissolution in 100 µL of methanol. Analytes were separated using a Zorbax Eclipse Plus C18 column under gradient elution with aqueous 10 mM NH4HCO3 (pH 8.0) and methanol as mobile phases. Matrix-matched calibrations allowed the assessment of DFSA drugs of quite different octanol–water partition coefficients (Ko/w), from 1.32 101 for pregabalin to 2.45 105 for clomipramine (Log P values from 1.12 (pregabalin) to 5.39 (clomipramine)). The limit of detection (LOD) was between 0.0075 to 0.37 µg L−1, with analytical recoveries ranging from 73 to 103%, and relative standard deviations (RSDs) within the 2–20% range. The applicability of the method was demonstrated after analysing urine samples under forensic investigation
PB Elsevier
SN 0021-9673
YR 2023
FD 2023
LK http://hdl.handle.net/10347/32911
UL http://hdl.handle.net/10347/32911
LA eng
NO Journal of Chromatography A, Volume 1706, 2023, 464284
NO This work was supported by the Dirección Xeral de I+D – Xunta de Galicia Grupos de Referencia Competitiva (project number ED431C2018/19)
DS Minerva
RD 24 abr 2026