title: Enantioselective determination of cathinone derivatives in human hair by capillary electrophoresis combined in-line with solid-phase extraction.
abstract: A suitable method has been developed and validated for the chiral separation and determination of R,S-mephedrone and one of its metabolites, R,S-4-methylephedrine, and R,S-methylenedioxypyrovalerone (R,S-MDPV) in human hair samples by the in-line coupling between SPE and CD-assisted CE with a previous sample pretreatment procedure based on pressurized liquid extraction. Optimum separation was achieved on a fused silica-capillary of 50 μm id and 80 cm total length using 12 mg/mL β-CD in an aqueous solution of 80 mM disodium phosphate at pH 2.5 as the BGE and an applied voltage of 30 kV. The SPE-CE device consists of a short length of a capillary of 2 mm packed with Oasis HLB sorbent, which was inserted near to the inlet end of the CE capillary. Several parameters affecting the in-line preconcentration were evaluated. The LOQs reached for hair samples were 0.05 ng/mg for the enantiomers of mephedrone and its metabolite, and 0.40 ng/mg for the enantiomers of MDPV. The RSDs (%) obtained in intra- and interday studies were less than 10% and the relative recoveries were greater than 80%. The method established in this paper is advantageous for its simplicity, overall analysis time and ability to provide information of both enantiomers of a chiral drug in hair samples.
authors.affiliation: Department of Analytical Chemistry and Organic Chemistry, Universitat Rovira i Virgili, Sescelades Campus, Marcel·lí Domingo, Tarragona, Spain.
authors.forename: Tatiana
authors.initials: T
authors.lastname: Baciu
authors.affiliation: Department of Analytical Chemistry and Organic Chemistry, Universitat Rovira i Virgili, Sescelades Campus, Marcel·lí Domingo, Tarragona, Spain.
authors.forename: Francesc
authors.initials: F
authors.lastname: Borrull
authors.affiliation: Department of Analytical Chemistry and Organic Chemistry, Universitat Rovira i Virgili, Sescelades Campus, Marcel·lí Domingo, Tarragona, Spain. marta.calull@urv.cat.
authors.forename: Marta
authors.initials: M
authors.lastname: Calull
authors.affiliation: Department of Analytical Chemistry and Organic Chemistry, Universitat Rovira i Virgili, Sescelades Campus, Marcel·lí Domingo, Tarragona, Spain.
authors.forename: Carme
authors.initials: C
authors.lastname: Aguilar
mesh_terms: D000470:Alkaloids / Q000032:analysis*; D019075:Electrophoresis, Capillary / Q000379:methods*; D006197:Hair / Q000737:chemistry*; D006801:Humans; D057230:Limit of Detection; D052616:Solid Phase Extraction / Q000379:methods*; D013237:Stereoisomerism; D013696:Temperature
chemical_list: D000470:Alkaloids; C023665:cathinone
keywords: Chiral CE; Hair analysis; In-line solid-phase extraction; Pressurized liquid extraction; Synthetic cathinones