ORIGINAL PAPER Chemical profile of meta-chlorophenylpiperazine (m-CPP) in ecstasy tablets by easy ambient sonic-spray ionization, X-ray fluorescence, ion mobility mass spectrometry and NMR Wanderson Romão & Priscila M. Lalli & Marcos F. Franco & Gustavo Sanvido & Nicolas V. Schwab & Rafael Lanaro & José Luiz Costa & Bruno D. Sabino & Maria Izabel M. S. Bueno & Gilberto F. de Sa & Romeu J. Daroda & Vanderlea de Souza & Marcos N. Eberlin Received: 18 November 2010 / Revised: 2 February 2011 / Accepted: 23 March 2011 / Published online: 9 April 2011 # Springer-Verlag 2011 Abstract Meta-chlorophenylpiperazine (m-CPP) is a new illicit drug that has been sold as ecstasy tablets. Easy ambient sonic-spray ionization mass spectrometry (EASI-MS) and X- ray fluorescence spectrometry (XRF) are shown to provide relatively simple and selective screening tools to distinguish m-CPP tablets from tablets containing amphetamines (mainly 3,4-methylenedioxymethamphetamine (MDMA)). EASI-MS detects the active ingredients in their protonated forms: [m-CPP+H] + of m/z 197, [MDMA+H] + of m/z 194, and [2MDMA+HCl+H] + of m/z 423 and other ions from excipients directly on the tablet surface, providing distinct chemical fingerprints. XRF identifies Cl, K, Ca, Fe, and Cu as inorganic ingredients present in the m-CPP tablets. In contrast, higher Cl concentrations and a more diverse set of elements (P, Cl, Ca, Fe, Cu, Zn, Pt, V, Hf, Ti, Pt, and Zr) were found in MDMA tablets. Principal component analysis applied to XRF data arranged samples in three groups: m-CPP tablets (four samples), MDMA tablets (twenty three sam- ples), and tablets with no active ingredients (three samples). The EASI-MS and XRF techniques were also evaluated to quantify m-CPP in ecstasy tablets, with concentrations ranging from 4 to 40 mg of m-CPP per tablets. The m-CPP could only be differentiated from its isomers (o-CPP and for the three isomers p-CPP) by traveling wave ion mobility mass spectrometry and NMR measurements. Keywords Drug monitoring/drug screening . Ambient mass spectrometry/EASI-MS . Forensics/toxicology . Metals/heavy metals . X-ray spectroscopy (XPS | XRF | EDX) . NMR/ESR Introduction Ecstasy is a well-known illicit drug with variable composition, but it usually contains 3,4-methylenedioxymethamphetamine (MDMA) as the main active ingredient. Recently, a new W. Romão (*) : P. M. Lalli : M. F. Franco : G. Sanvido : M. N. Eberlin ThoMSon Mass Spectrometry Laboratory, University of Campinas-UNICAMP, 13084-971 Campinas, SP, Brazil e-mail: wandersonromao@gmail.com N. V. Schwab : M. I. M. S. Bueno X-Ray Spectroscopy Group, Institute of Chemistry, University of Campinas-UNICAMP, 13084-971 Campinas, SP, Brazil R. Lanaro : J. L. Costa Poison Control Center–Faculty of Medical Sciences, University of Campinas-UNICAMP, 13084-971 Campinas, SP, Brazil B. D. Sabino Carlos Éboli Institute of Criminalistics, 20060-050 Rio de Janeiro, RJ, Brazil G. F. de Sa : R. J. Daroda : V. de Souza Division of Chemical Metrology, Directorate of Industrial and Scientific Metrology, National Institute of Metrology, Standardization and Industrial Quality, 25250-020 Duque de Caxias, RJ, Brazil G. F. de Sa Department of Fundamental Chemistry, Federal University of Pernambuco, 50.740-540 Recife, PE, Brazil Anal Bioanal Chem (2011) 400:3053–3064 DOI 10.1007/s00216-011-4883-9