title: Liquid chromatography tandem mass spectrometry determination of selected synthetic cathinones and two piperazines in oral fluid. Cross reactivity study with an on-site immunoassay device.
abstract: Since the past few years, several synthetic cathinones and piperazines have been introduced into the drug market to substitute illegal stimulant drugs such as amphetamine and derivatives or cocaine due to their unregulated situation. These emerging drugs are not usually included in routine toxicological analysis. We developed and validated a LC-MS/MS method for the determination of methedrone, methylone, mephedrone, 3,4-methylenedioxypyrovalerone (MDPV), fluoromethcathinone, fluoromethamphetamine, 1-(3-chlorophenyl)piperazine (mCPP) and 3-trifluoromethylphenylpiperazine (TFMPP) in oral fluid. Sample extraction was performed using Strata X cartridges. Chromatographic separation was achieved in 10min using an Atlantis(®) T3 column (100mm×2.1mm, 3μm), and formic acid 0.1% and acetonitrile as mobile phase. The method was satisfactorily validated, including selectivity, linearity (0.2-0.5 to 200ng/mL), limits of detection (0.025-0.1ng/mL) and quantification (0.2-0.5ng/mL), imprecision and accuracy in neat oral fluid (%CV=0.0-12.7% and 84.8-103.6% of target concentration, respectively) and in oral fluid mixed with Quantisal™ buffer (%CV=7.2-10.3% and 80.2-106.5% of target concentration, respectively), matrix effect in neat oral fluid (-11.6 to 399.7%) and in oral fluid with Quantisal™ buffer (-69.9 to 131.2%), extraction recovery (87.9-134.3%) and recovery from the Quantisal™ (79.6-107.7%), dilution integrity (75-99% of target concentration) and stability at different conditions (-14.8 to 30.8% loss). In addition, cross reactivity produced by the studied synthetic cathinones in oral fluid using the Dräger DrugTest 5000 was assessed. All the analytes produced a methamphetamine positive result at high concentrations (100 or 10μg/mL), and fluoromethamphetamine also at low concentration (0.075μg/mL).
authors.affiliation: Servicio de Toxicología Forense, Instituto de Ciencias Forenses, Universidad de Santiago de Compostela, San Francisco s/n, 15782 Santiago de Compostela, Spain. Electronic address: ana.decastro@usc.es.
authors.forename: Ana
authors.initials: A
authors.lastname: de Castro
authors.affiliation: Servicio de Toxicología Forense, Instituto de Ciencias Forenses, Universidad de Santiago de Compostela, San Francisco s/n, 15782 Santiago de Compostela, Spain. Electronic address: elena.lendoiro@usc.es.
authors.forename: Elena
authors.initials: E
authors.lastname: Lendoiro
authors.affiliation: Servicio de Toxicología Forense, Instituto de Ciencias Forenses, Universidad de Santiago de Compostela, San Francisco s/n, 15782 Santiago de Compostela, Spain. Electronic address: hadrianoia@hotmail.com.
authors.forename: Hadriana
authors.initials: H
authors.lastname: Fernández-Vega
authors.affiliation: Drug Testing Solutions & Forensic Applications, Dräger Safety AG & Co. KGaA, Lübeck, Germany. Electronic address: stefan.Steinmeyer@draeger.com.
authors.forename: Stefan
authors.initials: S
authors.lastname: Steinmeyer
authors.affiliation: Servicio de Toxicología Forense, Instituto de Ciencias Forenses, Universidad de Santiago de Compostela, San Francisco s/n, 15782 Santiago de Compostela, Spain. Electronic address: manuel.lopez-rivadulla@usc.es.
authors.forename: Manuel
authors.initials: M
authors.lastname: López-Rivadulla
authors.affiliation: Servicio de Toxicología Forense, Instituto de Ciencias Forenses, Universidad de Santiago de Compostela, San Francisco s/n, 15782 Santiago de Compostela, Spain. Electronic address: angelines.cruz@usc.es.
authors.forename: Angelines
authors.initials: A
authors.lastname: Cruz
mesh_terms: D000470:Alkaloids / Q000032:analysis* / Q000138:chemical synthesis; D002138:Calibration; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003429:Cross Reactions; D006801:Humans; D007118:Immunoassay; D010879:Piperazines / Q000032:analysis*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D000470:Alkaloids; D010879:Piperazines; C023665:cathinone
keywords: Immunoassay cross reactivity; LC–MS/MS; Oral fluid; Synthetic cathinone; Synthetic piperazine