Abstract
The detection of new psychoactive substances (NPS) in hair proved to provide insight into their current diffusion among the population and the social characteristics of these synthetic drugs’ users. Therefore, a UHPLC–MS/MS method was developed in order to determine 31 stimulant and psychedelic substituted phenethylamines, and dissociative drugs in hair samples. The method proved to be simple, fast, specific, and sensitive. The absence of matrix interferents, together with excellent repeatability of both retention times and relative abundances of diagnostic transitions, allowed the correct identification of all analytes tested. The method showed optimal linearity in the interval 10–1000 pg/mg, with correlation coefficient values varying between 0.9981 and 0.9997. Quantitation limits ranged from 1.8 pg/mg for 4-methoxyphencyclidine (4-MeO-PCP) up to 35 pg/mg for 6-(2-aminopropyl)benzofuran (6-APB). The method was applied to (i) 23 real samples taken from proven MDMA and ketamine abusers and (ii) 54 real hair samples which had been previously tested negative during regular drug screening in driver’s license recovery. Six samples tested positive for at least one target analyte. Methoxetamine (MXE) was found in three cases (range of concentration 7.7–27 pg/mg); mephedrone (4-MMC) was found in two cases (50–59 pg/mg) while one sample tested positive for methylone at 28 pg/mg. Other positive findings included 4-methylethcathinone (4-MEC), alpha-pyrrolidinovalerophenone (α-PVP), 4-fluoroamphetamine (4-FA), 3,4-methylenedioxypyrovalerone (MDPV), and diphenidine. The present study confirms the increasing diffusion of new designer drugs with enhanced stimulant activity among the target population of poly-abuse consumers.
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References
Davidson C. New psychoactive substances. Prog Neuropsychopharmacol Biol Psychiatry. 2012;39:219–20.
King L, Kicman T. A brief history of “new psychoactive substances”. Drug Test Anal. 2011;3:401–3.
Favretto D, Pascali JP, Tagliaro F. New challenges and innovation in forensic toxicology: focus on the “new psychoactive substances”. J Chromatogr A. 2013;1287:84–95.
Kintz P, Salomone A, Vincenti M. Hair analysis in clinical and forensic toxicology. USA: Academic; 2015.
Vardakou I, Pistos C, Spiliopoulou C. Spice drugs as a new trend: mode of action, identification and legislation. Toxicol Lett. 2010;197:157–62.
Salomone A, Luciano C, Di Corcia D, Gerace E, Vincenti M. Hair analysis as a tool to evaluate the prevalence of synthetic cannabinoids in different populations of drug consumers. Drug Test Anal. 2014;6:126–34.
Kerwin J. Doors of deception: the diaspora of designer drugs. Drug Test Anal. 2011;3:527–31.
Papanti D, Schifano F, Botteon G, Bertossi F, Mannix J, Vidoni D, et al. “Spiceophrenia”: a systematic overview of “spice”-related psychopathological issues and a case report. Hum Psychopharmacol. 2013;28:379–89.
Crews B. Synthetic cannabinoids. The challenges of testing for designer drugs. http://www.aacc.org/publications/cln/2013/february/Pages/Cannabinoids.aspx# (2013).
Hutter M, Kneisel S, Auwärter V, Neukamm M. Determination of 22 synthetic cannabinoids in human hair by liquid chromatography-tandem mass spectrometry. J Chromatogr B Anal Technol Biomed Life Sci. 2012;903:95–101.
Salomone A, Gerace E, D’Urso F, Di Corcia D, Vincenti M. Simultaneous analysis of several synthetic cannabinoids, THC, CBD and CBN, in hair by ultra-high performance liquid chromatography tandem mass spectrometry. Method validation and application to real samples. J Mass Spectrom. 2012;47:604–10.
Strano-Rossi S, Odoardi S, Fisichella M, Anzillotti L, Gottardo R, Tagliaro F. Screening for new psychoactive substances in hair by ultrahigh performance liquid chromatography-electrospray ionization tandem mass spectrometry. J Chromatogr A. 2014;1372C:145–56.
Gottardo R, Sorio D, Musile G, Trapani E, Seri C, Serpelloni G, et al. Screening for synthetic cannabinoids in hair by using LC-QTOF MS: a new and powerful approach to study the penetration of these new psychoactive substances in the population. Med Sci Law. 2014;54:22–7.
Torrance H, Cooper G. The detection of mephedrone (4-methylmethcathinone) in 4 fatalities in Scotland. Forensic Sci Int. 2010;202:e62–3.
Barroso M, Costa S, Dias M, Vieira DN, Queiroz J, López-Rivadulla M. Analysis of phenylpiperazine-like stimulants in human hair as trimethylsilyl derivatives by gas chromatography–mass spectrometry. J Chromatogr A. 2010;1217:6274–80.
Kikura-Hanajiri R, Kawamura M, Saisho K, Kodama Y, Goda Y. The disposition into hair of new designer drugs; methylone, MBDB and methcathinone. J Chromatogr B Anal Technol Biomed Life Sci. 2007;855:121–6.
Martin M, Muller JF, Turner K, Duez M, Cirimele V. Evidence of mephedrone chronic abuse through hair analysis using GC/MS. Forensic Sci Int. 2012;218:44–8.
Gerace E, Petrarulo M, Bison F, Salomone A, Vincenti M. Toxicological findings in a fatal multidrug intoxication involving mephedrone. Forensic Sci Int. 2014;243C:68–73.
Kim JY, Jung KS, Kim MK, Lee JI, In MK. Simultaneous determination of psychotropic phenylalkylamine derivatives in human hair by gas chromatography / mass spectrometry. Rapid Commun Mass Spectrom. 2007:1705–20
Namera A, Konuma K, Saito T, Ota S, Oikawa H, Miyazaki S, et al. Simple segmental hair analysis for α-pyrrolidinophenone-type designer drugs by MonoSpin extraction for evaluation of abuse history. J Chromatogr B Anal Technol Biomed Life Sci. 2013;942–943:15–20.
Namera A, Urabe S, Saito T, Torikoshi-Hatano A, Shiraishi H, Arima Y, et al. A fatal case of 3,4-methylenedioxypyrovalerone poisoning: coexistence of α-pyrrolidinobutiophenone and α-pyrrolidinovalerophenone in blood and/or hair. Forensic Toxicol. 2013;31:338–43.
Shah SB, Deshmukh NIK, Barker J, Petróczi A, Cross P, Archer R, et al. Quantitative analysis of mephedrone using liquid chromatography tandem mass spectroscopy: application to human hair. J Pharm Biomed Anal. 2012;61:64–9.
Rust KY, Baumgartner MR, Dally AM, Kraemer T. Prevalence of new psychoactive substances: a retrospective study in hair. Drug Test Anal. 2012;4:402–8.
Wikström M, Thelander G, Nyström I, Kronstrand R. Two fatal intoxications with the new designer drug methedrone (4-methoxymethcathinone) autopsy cases. J Anal Toxicol. 2010;34:594–8.
Lendoiro E, Jiménez-Morigosa C, Cruz A, López-Rivadulla M, de Castro A. O20: Hair analysis of amphetamine-type stimulant drugs (ATS), including synthetic cathinones and piperazines, by LC-MSMS. Toxicol Anal Clin. 2014;26:S13.
Di Corcia D, D’Urso F, Gerace E, Salomone A, Vincenti M. Simultaneous determination in hair of multiclass drugs of abuse (including THC) by ultra-high performance liquid chromatography–tandem mass spectrometry. J Chromatogr B. 2012;899:154–9.
Hubaux A, Vos G. Decision and detection limits for calibration curves. Anal Chem. 1970;42:849–55.
Stanczuk A, Morris N, Gardner E, Kavanagh P. Identification of (2-aminopropyl)benzofuran (APB) phenyl ring positional isomers in Internet purchased products. Drug Test Anal. 2013;5:270–6.
Brandt SD, Daley PF, Cozzi NV. Analytical characterization of three trifluoromethyl-substituted methcathinone isomers. Drug Test Anal. 2012;4:525–9.
Power JD, McGlynn P, Clarke K, McDermott SD, Kavanagh P, O’Brien J. The analysis of substituted cathinones. Part 1: Chemical analysis of 2-, 3- and 4-methylmethcathinone. Forensic Sci Int. 2011;212:6–12.
Marinetti LJ, Antonides HM. Analysis of synthetic cathinones commonly found in bath salts in human performance and postmortem toxicology: method development, drug distribution and interpretation of results. J Anal Toxicol. 2013;37:135–46.
Hondebrink L, Nugteren-van Lonkhuyzen JJ, Van Der Gouwe D, Brunt TM. Monitoring new psychoactive substances (NPS) in The Netherlands: data from the drug market and the Poisons Information Centre. Drug Alcohol Depend. 2015;147:109–15.
Adamowicz P, Tokarczyk B, Stanaszek R, Slopianka M. Fatal mephedrone intoxication—a case report. J Anal Toxicol. 2013;37:37–42.
Hasegawa K, Wurita A, Minakata K, Gonmori K, Nozawa H, Yamagishi I, et al. Postmortem distribution of AB-CHMINACA, 5-fluoro-AMB, and diphenidine in body fluids and solid tissues in a fatal poisoning case: usefulness of adipose tissue for detection of the drugs in unchanged forms. Forensic Toxicol. 2015;33:45–53.
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Salomone, A., Gazzilli, G., Di Corcia, D. et al. Determination of cathinones and other stimulant, psychedelic, and dissociative designer drugs in real hair samples. Anal Bioanal Chem 408, 2035–2042 (2016). https://doi.org/10.1007/s00216-015-9247-4
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DOI: https://doi.org/10.1007/s00216-015-9247-4