Author, as appears in the article.: Pérez-Alcaraz A; Borrull F; Aguilar C; Calull M; Benavente F
Department: Química Analítica i Química Orgànica
URV's Author/s: Aguilar Anguera, Maria del Carmen / Borrull Ballarín, Francesc / Calull Blanch, Marta
Keywords: Uv Urine analysis Synthetic cathinones Sulphated cyclodextrins Separation Resolution Methylenedioxypyrovalerone mdpv In-line preconcentration Enantiodetermination in-line preconcentration Enantiodetermination Dopamine Derivatives Cyclodextrin Cathinones Capillary electrophoresis mass spectrometry Amphetamine-type stimulants
Abstract: © 2020 Elsevier B.V. This study presents for the first time an in-line solid-phase extraction capillary electrophoresis-mass spectrometry (SPE-CE-MS) method for the enantiodetermination of drugs of abuse in urine samples. The enantioseparation of R,S-3,4-methylenedioxypyrovalerone (R,S-MDPV) was achieved with a 10 mM ammonium acetate BGE (pH 7) that contained 0.5% (m/v) of sulphated-α-CD as chiral selector. At these pH conditions, this CD was negatively charged, which prevented its entrance into the mass spectrometer since it migrates in the opposite direction. To improve sensitivity, an in-line SPE-CE-MS method using high pressure for sample introduction (i.e. 20 min at 3 bars) was developed. Furthermore, the conditioning procedure and the first part of the electrophoretic separation were performed by switching off the nebulizer gas and the ionization source voltage to avoid non-volatile contaminant arrival into the mass spectrometer. The developed methodology was validated by analyzing urine samples, which required a very simple liquid-liquid extraction (LLE) sample pretreatment. Linearity ranged from 30 to 250 ng mL−1, limit of detection (LOD) was 10 ng mL−1, relative standard deviation (RSD) values were below 10.5% in terms of intra-day and inter-day precision and the relative error values were below 9% for peak areas accuracy.
Thematic Areas: Zootecnia / recursos pesqueiros Spectroscopy Saúde coletiva Química Nutrição Medicina veterinaria Medicina iii Medicina ii Medicina i Materiais Interdisciplinar Geociências General medicine General chemistry Farmacia Ensino Engenharias iv Engenharias iii Engenharias ii Engenharias i Ciências biológicas iii Ciências biológicas ii Ciências biológicas i Ciências ambientais Ciências agrárias i Ciência de alimentos Chemistry, analytical Chemistry (miscellaneous) Biotecnología Biodiversidade Biochemistry Astronomia / física Analytical chemistry Administração pública e de empresas, ciências contábeis e turismo
licence for use: https://creativecommons.org/licenses/by/3.0/es/
ISSN: 0039-9140
Author's mail: carme.aguilar@urv.cat marta.calull@urv.cat francesc.borrull@urv.cat
Author identifier: 0000-0002-5913-2599 0000-0002-5258-1949 0000-0003-2718-9336
Record's date: 2024-07-27
Papper version: info:eu-repo/semantics/acceptedVersion
Link to the original source: https://www.sciencedirect.com/science/article/abs/pii/S0039914020312856?via%3Dihub
Licence document URL: https://repositori.urv.cat/ca/proteccio-de-dades/
Papper original source: Talanta. 225 (121994): 121994-
APA: Pérez-Alcaraz A; Borrull F; Aguilar C; Calull M; Benavente F (2021). Enantiodetermination of R,S-3,4-methylenedioxypyrovalerone in urine samples by high pressure in-line solid-phase extraction capillary electrophoresis-mass spectrometry. Talanta, 225(121994), 121994-. DOI: 10.1016/j.talanta.2020.121994
Article's DOI: 10.1016/j.talanta.2020.121994
Entity: Universitat Rovira i Virgili
Journal publication year: 2021
Publication Type: Journal Publications