title: Determination of amphetamine-type stimulants in oral fluid by solid-phase microextraction and gas chromatography-mass spectrometry.
abstract: A method for the simultaneous identification and quantification of amphetamine (AMP), methamphetamine (MET), fenproporex (FEN), diethylpropion (DIE) and methylphenidate (MPH) in oral fluid collected with Quantisal™ device has been developed and validated. Thereunto, in-matrix propylchloroformate derivatization followed by direct immersion solid-phase microextraction and gas chromatography-mass spectrometry were employed. Deuterium labeled AMP was used as internal standard for all the stimulants and analysis was performed using the selected ion monitoring mode. The detector response was linear for the studied drugs in the concentration range of 2-256 ng mL(-1) (neat oral fluid), except for FEN, whereas the linear range was 4-256 ng mL(-1). The detection limits were 0.5 ng mL(-1) (MET), 1 ng mL(-1) (MPH) and 2 ng mL(-1) (DIE, AMP, FEN), respectively. Accuracy of quality control samples remained within 98.2-111.9% of the target concentrations, while precision has not exceeded 15% of the relative standard deviation. Recoveries with Quantisal™ device ranged from 77.2% to 112.1%. Also, the goodness-of-fit concerning the ordinary least squares model in the statistical inference of data has been tested through residual plotting and ANOVA. The validated method can be easily automated and then used for screening and confirmation of amphetamine-type stimulants in drivers' oral fluid.
authors.affiliation: Setor Técnico-Científico, Superintendência Regional do Departamento de Polícia Federal no Rio Grande do Sul, Porto Alegre, Brazil. daniele.dzs@dpf.gov.br
authors.forename: Daniele Z
authors.initials: DZ
authors.lastname: Souza
authors.forename: Paula O
authors.initials: PO
authors.lastname: Boehl
authors.forename: Eloisa
authors.initials: E
authors.lastname: Comiran
authors.forename: Kristiane C
authors.initials: KC
authors.lastname: Mariotti
authors.forename: Flavio
authors.initials: F
authors.lastname: Pechansky
authors.forename: Paulina C A V
authors.initials: PC
authors.lastname: Duarte
authors.forename: Raquel
authors.initials: R
authors.lastname: De Boni
authors.forename: Pedro E
authors.initials: PE
authors.lastname: Froehlich
authors.forename: Renata P
authors.initials: RP
authors.lastname: Limberger
mesh_terms: D000661:Amphetamine / Q000032:analysis*; D000662:Amphetamines / Q000032:analysis; D000697:Central Nervous System Stimulants / Q000032:analysis*; D004053:Diethylpropion / Q000032:analysis; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D057230:Limit of Detection; D008694:Methamphetamine / Q000032:analysis; D008774:Methylphenidate / Q000032:analysis; D012463:Saliva / Q000737:chemistry*; D052617:Solid Phase Microextraction / Q000379:methods*
chemical_list: D000662:Amphetamines; D000697:Central Nervous System Stimulants; D008774:Methylphenidate; D008694:Methamphetamine; D000661:Amphetamine; D004053:Diethylpropion; C026013:fenproporex