title: Determination of ketamine, norketamine and dehydronorketamine in urine by hollow-fiber liquid-phase microextraction using an essential oil as supported liquid membrane.
abstract: Here, we present a method for the determination of ketamine (KT) and its main metabolites, norketamine (NK) and dehydronorketamine (DHNK) in urine samples by using hollow-fiber liquid-phase microextraction (HF-LPME) in the three-phase mode. The fiber pores were filled with eucalyptus essential oil and a solution of 1.0mol/L of HCl was introduced into the lumen of the fiber (acceptor phase). The fiber was submersed in the alkalinized urine containing 10% NaCl, and the system was submitted to lateral shaking (2400rpm) during 30min. Acceptor phase was withdrawn from the fiber, dried and the residue was then derivatized with trifluoroacetic anhydride (TFAA) for further determination by gas chromatography-mass spectrometry (GC-MS). The calibration curves were linear over the specified range and limits of detection (LoDs) obtained for KT, NK and DHNK were below the cut-off value (1.0ng/mL) recommended by the United Nations Office on Drugs and Crime (UNODC). A totally "green chemistry" approach of the sample extraction was obtained by using essential oil as a supported liquid membrane in HF-LPME. The developed method was successfully validated and applied to urine samples collected from two clinical cases in which KT was suspected to be involved.
authors.affiliation: Faculty of Pharmaceutical Sciences, University of São Paulo, São Paulo, Brazil. Electronic address: andrebairros@yahoo.com.br.
authors.forename: André Valle de
authors.initials: AV
authors.lastname: Bairros
authors.affiliation: Campinas Poison Control Center, Faculty of Medical Sciences, State University of Campinas, Campinas, Brazil.
authors.forename: Rafael
authors.initials: R
authors.lastname: Lanaro
authors.affiliation: Faculty of Pharmaceutical Sciences, University of São Paulo, São Paulo, Brazil.
authors.forename: Rafael Menck de
authors.initials: RM
authors.lastname: Almeida
authors.affiliation: Faculty of Pharmaceutical Sciences, University of São Paulo, São Paulo, Brazil.
authors.forename: Mauricio
authors.initials: M
authors.lastname: Yonamine
mesh_terms: D000778:Anesthetics, Dissociative / Q000652:urine*; D005052:Eucalyptus; D053593:Forensic Toxicology / Q000379:methods; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D006851:Hydrochloric Acid; D007649:Ketamine / Q000031:analogs & derivatives* / Q000652:urine*; D057230:Limit of Detection; D059627:Liquid Phase Microextraction / Q000379:methods*; D010938:Plant Oils
chemical_list: D000778:Anesthetics, Dissociative; D010938:Plant Oils; D007649:Ketamine; D006851:Hydrochloric Acid; C033419:norketamine
keywords: Essential oils; Gas chromatography–mass spectrometry; Hollow fiber–liquid phase microextraction; Ketamine; Urine