title: An LC-MS/MS methodological approach to the analysis of hair for amphetamine-type-stimulant (ATS) drugs, including selected synthetic cathinones and piperazines.
abstract: Amphetamine-type-stimulants (ATS) are the second most commonly used group of illicit drugs worldwide. However, in the last few years, new psychoactive substances (NPS) with stimulant effects have appeared on the illegal market, which are not detected with traditional analytical methods. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination in hair of classic ATS (amphetamine, methamphetamine, 3,4-methylenedioxymethamphetamine and 3,4-methylenedioxyamphetamine), synthetic cathinones (methylone, methedrone, mephedrone, 3,4-methylenedioxypyrovalerone, (±)-4-fluoromethamphetamine and 4-fluoromethcathinone), synthetic piperazines (1-(3-chlorophenyl)piperazine (mCPP) and 3-trifluoromethylphenylpiperazine), and medicines (trazodone and phenazone) that produce mCPP as a metabolite, was developed and fully validated. Hair samples (30 mg) were incubated in acid methanol (0.1% HCl) and extracted by a mixed-mode solid-phase extraction. Chromatographic separation was performed using an Atlantis T3 (3 µm; 2.1x50 mm) analytical column, and ammonium formate 2 mM pH 3 and acetonitrile as mobile phase. The method was validated, including selectivity (no endogenous or exogenous interferences); linearity (2-20 to 2000-4000 pg/mg); limits of detection (0.2 to 5 pg/mg) and quantification (2 to 20 pg/mg); accuracy (93.4-109.4% of target concentration); imprecision (%CV<11.6%); extraction recovery (40.5-92.1%); matrix effect (24.1-227.2%); process efficiency (9.8-165.7%) and stability in the autosampler (-14.5% of loss). The method was applied to the analysis of 16 hair samples. Amphetamine (n=7; 69.1-777.1 pg/mg), methamphetamine (n=3; 120.4-1,538.9 pg/mg), MDA (n=2; 27.8-135.4 pg/mg) and MDMA (n=8; 73.4-3,654.5 pg/mg) were found. Moreover, 10 positive results for mCPP were detected (341.7->4000 pg/mg); however, in all cases trazodone identification (2085.3->4000 pg/mg) probed a licit origin of mCPP. Copyright © 2016 John Wiley & Sons, Ltd.
authors.affiliation: Servicio de Toxicología, Instituto de Ciencias Forenses, Universidad de Santiago de Compostela, San Francisco s/n, 15782, Santiago de Compostela, Spain.
authors.forename: Elena
authors.initials: E
authors.lastname: Lendoiro
authors.affiliation: Servicio de Toxicología, Instituto de Ciencias Forenses, Universidad de Santiago de Compostela, San Francisco s/n, 15782, Santiago de Compostela, Spain.
authors.forename: Cristian
authors.initials: C
authors.lastname: Jiménez-Morigosa
authors.affiliation: Servicio de Toxicología, Instituto de Ciencias Forenses, Universidad de Santiago de Compostela, San Francisco s/n, 15782, Santiago de Compostela, Spain.
authors.forename: Angelines
authors.initials: A
authors.lastname: Cruz
authors.affiliation: Servizo de Psiquiatría, Complexo Hospitalario Universitario de Santiago (CHUS), Servizo Galego de Saúde (SERGAS), Santiago de Compostela, Spain.
authors.forename: Mario
authors.initials: M
authors.lastname: Páramo
authors.affiliation: Servicio de Toxicología, Instituto de Ciencias Forenses, Universidad de Santiago de Compostela, San Francisco s/n, 15782, Santiago de Compostela, Spain.
authors.forename: Manuel
authors.initials: M
authors.lastname: López-Rivadulla
authors.affiliation: Servicio de Toxicología, Instituto de Ciencias Forenses, Universidad de Santiago de Compostela, San Francisco s/n, 15782, Santiago de Compostela, Spain.
authors.forename: Ana
authors.initials: A
authors.lastname: de Castro
mesh_terms: D000470:Alkaloids / Q000032:analysis*; D000662:Amphetamines / Q000032:analysis*; D000697:Central Nervous System Stimulants / Q000032:analysis*; D002853:Chromatography, Liquid / Q000379:methods; D005260:Female; D006197:Hair / Q000737:chemistry*; D006801:Humans; D013287:Illicit Drugs / Q000032:analysis*; D057230:Limit of Detection; D008297:Male; D010879:Piperazines / Q000032:analysis*; D015813:Substance Abuse Detection / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods
chemical_list: D000470:Alkaloids; D000662:Amphetamines; D000697:Central Nervous System Stimulants; D013287:Illicit Drugs; D010879:Piperazines; C023665:cathinone
keywords: amphetamine-type-stimulants; hair; new psychoactive substances; synthetic cathinones; synthetic piperazines