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Analytical strategy to investigate 3,4-methylenedioxypyrovalerone (MDPV) metabolites in consumers’ urine by high-resolution mass spectrometry

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Abstract

The potential of high-resolution mass spectrometry (HRMS) for the investigation of human in vivo metabolism of 3,4-methylenedioxypyrovalerone (MDPV) using urine collected from a consumer (this is, in non-controlled experiments) has been investigated. As a control sample was not available, the common approach based on the comparison of a control/blank sample and samples collected after drug intake could not be used. Alternatively, an investigation based on common fragmentation pathways was applied, assuming that most metabolites share some fragments with the parent drug. An extension of this approach was also applied based on the fragmentation pathway of those metabolites identified in urine samples in the first step. The use of MSE experiments (sequential acquisition of mass spectra at low and high collision energy) has been crucial to this aim as it allowed promoting fragmentation in the collision cell without any previous precursor ion selection. MDPV belongs to the group of new psychoactive substances (NPS), being known as the “cannibal drug”. This substance is being abused more and more and is associated with dangerous side effects. The human metabolites (both phase I and phase II) were detected and tentatively identified by accurate mass full-spectrum measurements using ultra-high performance liquid chromatography coupled to hybrid quadrupole time-of-flight mass spectrometry (UHPLC-QTOF MS). Following this strategy, up to 10 phase I metabolites, together with some glucuronides and sulphates, were detected and tentative structures were proposed. Several compounds identified in this work have not been previously reported in the literature.

Detection of metabolites of MDPV by common fragmentation pathway

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Acknowledgments

The authors acknowledge the financial support of the Spanish Ministry of Economy and Competitiveness (CTQ2012-36189) and of Generalitat Valenciana (research group of excellence PROMETEOII/2014/023; ISIC Envi-Food 2014/016). Spanish Health National System is acknowledged for O. J. Pozo contract (MS10/00576).

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Correspondence to María Ibáñez.

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Ibáñez, M., Pozo, Ó.J., Sancho, J.V. et al. Analytical strategy to investigate 3,4-methylenedioxypyrovalerone (MDPV) metabolites in consumers’ urine by high-resolution mass spectrometry. Anal Bioanal Chem 408, 151–164 (2016). https://doi.org/10.1007/s00216-015-9088-1

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