Journal
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
Volume 400, Issue 9, Pages 3053-3064Publisher
SPRINGER HEIDELBERG
DOI: 10.1007/s00216-011-4883-9
Keywords
Drug monitoring/drug screening; Ambient mass spectrometry/EASI-MS; Forensics/toxicology; Metals/heavy metals; X-ray spectroscopy (XPS vertical bar XRF vertical bar EDX); NMR/ESR
Funding
- FAPESP [2009/07168-9, 2007/54357-6]
- CNPq [576183/2008-3]
- FAPERJ [E-26/190.060/2008]
- FINEP
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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 samples), 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.
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