PMID- 37572537 OWN - NLM STAT- MEDLINE DCOM- 20230823 LR - 20230823 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1706 DP - 2023 Sep 13 TI - 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. PG - 464284 LID - S0021-9673(23)00509-5 [pii] LID - 10.1016/j.chroma.2023.464284 [doi] 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 muL 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 (N(2) stream) and re-dissolution in 100 microL of methanol. Analytes were separated using a Zorbax Eclipse Plus C18 column under gradient elution with aqueous 10 mM NH(4)HCO(3) (pH 8.0) and methanol as mobile phases. Matrix-matched calibrations allowed the assessment of DFSA drugs of quite different octanol-water partition coefficients (K(o/w)), from 1.32 10(1) for pregabalin to 2.45 10(5) 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 microg 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. CI - Copyright (c) 2023 Elsevier B.V. All rights reserved. FAU - Justo-Vega, Ana AU - Justo-Vega A AD - Trace Element, Spectroscopy and Speciation Group (GETEE), Institute of Materials iMATUS, Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, Universidade de Santiago de Compostela, Avenida das Ciencias, s/n., Santiago de Compostela 15782, Spain. FAU - Jinadasa, Kamal K AU - Jinadasa KK AD - Trace Element, Spectroscopy and Speciation Group (GETEE), Institute of Materials iMATUS, Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, Universidade de Santiago de Compostela, Avenida das Ciencias, s/n., Santiago de Compostela 15782, Spain. FAU - Jayasinghe, G D Thilini Madurangika AU - Jayasinghe GDTM AD - Trace Element, Spectroscopy and Speciation Group (GETEE), Institute of Materials iMATUS, Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, Universidade de Santiago de Compostela, Avenida das Ciencias, s/n., Santiago de Compostela 15782, Spain. FAU - Alvarez-Freire, Ivan AU - Alvarez-Freire I AD - Forensic Sciences Institute "Luis Concheiro" (INCIFOR), Department of Pathologic Anatomy and Forensic Sciences, Faculty of Medicine, Universidade de Santiago de Compostela, Rua de San Francisco, s/n, Santiago de Compostela 15782, Spain. FAU - Bermejo, Ana Maria AU - Bermejo AM AD - Forensic Sciences Institute "Luis Concheiro" (INCIFOR), Department of Pathologic Anatomy and Forensic Sciences, Faculty of Medicine, Universidade de Santiago de Compostela, Rua de San Francisco, s/n, Santiago de Compostela 15782, Spain. FAU - Bermejo-Barrera, Pilar AU - Bermejo-Barrera P AD - Trace Element, Spectroscopy and Speciation Group (GETEE), Institute of Materials iMATUS, Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, Universidade de Santiago de Compostela, Avenida das Ciencias, s/n., Santiago de Compostela 15782, Spain. FAU - Moreda-Pineiro, Antonio AU - Moreda-Pineiro A AD - Trace Element, Spectroscopy and Speciation Group (GETEE), Institute of Materials iMATUS, Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, Universidade de Santiago de Compostela, Avenida das Ciencias, s/n., Santiago de Compostela 15782, Spain. Electronic address: antonio.moreda@usc.es. LA - eng PT - Journal Article DEP - 20230805 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - Y4S76JWI15 (Methanol) RN - NUV44L116D (Clomipramine) RN - 55JG375S6M (Pregabalin) RN - 0 (Solvents) SB - IM MH - *Tandem Mass Spectrometry/methods MH - Chromatography, High Pressure Liquid/methods MH - *Methanol MH - Clomipramine MH - Pregabalin MH - Chromatography, Liquid MH - Solvents/chemistry MH - Solid Phase Extraction OTO - NOTNLM OT - Drug-facilitated sexual assault OT - Membrane assisted solvent extraction OT - Urine COIS- Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper. EDAT- 2023/08/13 00:44 MHDA- 2023/08/23 06:42 CRDT- 2023/08/12 18:06 PHST- 2023/01/18 00:00 [received] PHST- 2023/03/24 00:00 [revised] PHST- 2023/08/04 00:00 [accepted] PHST- 2023/08/23 06:42 [medline] PHST- 2023/08/13 00:44 [pubmed] PHST- 2023/08/12 18:06 [entrez] AID - S0021-9673(23)00509-5 [pii] AID - 10.1016/j.chroma.2023.464284 [doi] PST - ppublish SO - J Chromatogr A. 2023 Sep 13;1706:464284. doi: 10.1016/j.chroma.2023.464284. Epub 2023 Aug 5.