title: Screening for illicit drugs in pooled human urine and urinated soil samples and studies on the stability of urinary excretion products of cocaine, MDMA, and MDEA in wastewater by hyphenated mass spectrometry techniques.
abstract: Monitoring population drug use through wastewater-based epidemiology (WBE) is a useful method to quantitatively follow trends and estimate total drug consumption in communities. Concentrations of drug biomarkers might be low in wastewater due to dilution; and therefore analysis of pooled urine (PU) is useful to detect consumed drugs and identify targets of illicit drugs use. The aims of the study were (1) to screen PU and urinated soil (US) samples collected at festivals for illicit drug excretion products using hyphenated techniques; (2) to develop and validate a hydrophilic interaction liquid chromatography - mass spectrometry / mass spectrometry (HILIC-MS/MS) method of quantifying urinary targets of identified drugs in wastewater; and (3) to conduct a 24 h stability study, using PU and US to better reflect the chemical environment for targets in wastewater. Cocaine (COC) and ecstasy-like compounds were the most frequently detected illicit drugs; an analytical method was developed to quantify their excretion products. Hydroxymethoxymethamphetamine (HMMA), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA), HMMA sulfate (HMMA-S), benzoylecgonine (BE), and cocaethylene (CE) had 85-102% of initial concentration after 8 h of incubation, whereas COC and ecgonine methyl ester (EME) had 74 and 67% after 8 h, respectively. HMMA showed a net increase during 24 h of incubation (107% ± 27, n = 8), possibly due to the cleavage of HMMA conjugates, and biotransformation of MDMA. The results suggest HMMA as analytical target for MDMA consumption in WBE, due to its stability in wastewater and its excretion as the main phase I metabolite of MDMA. Copyright © 2016 John Wiley & Sons, Ltd.
authors.affiliation: Department of Experimental and Clinical Toxicology, Institute of Experimental and Clinical Pharmacology and Toxicology, Saarland University, Homburg, Germany.
authors.forename: Marie
authors.initials: M
authors.lastname: Mardal
authors.affiliation: Toxicological Center, Department of Pharmaceutical Sciences, University of Antwerp, Antwerp, Belgium.
authors.forename: Juliet
authors.initials: J
authors.lastname: Kinyua
authors.affiliation: Department of Environmental Engineering, Technical University of Denmark, Kongens Lyngby, Denmark.
authors.forename: Pedram
authors.initials: P
authors.lastname: Ramin
authors.affiliation: TICTAC Communications Ltd, St George's, University of London, London, SW17 0RE, UK.
authors.forename: Bram
authors.initials: B
authors.lastname: Miserez
authors.affiliation: Toxicological Center, Department of Pharmaceutical Sciences, University of Antwerp, Antwerp, Belgium.
authors.forename: Alexander L N
authors.initials: AL
authors.lastname: Van Nuijs
authors.affiliation: Toxicological Center, Department of Pharmaceutical Sciences, University of Antwerp, Antwerp, Belgium.
authors.forename: Adrian
authors.initials: A
authors.lastname: Covaci
authors.affiliation: Department of Experimental and Clinical Toxicology, Institute of Experimental and Clinical Pharmacology and Toxicology, Saarland University, Homburg, Germany.|Department of Pharmacology and Pharmacoepidemiology, Heidelberg University Hospital, Heidelberg, Germany.
authors.forename: Markus R
authors.initials: MR
authors.lastname: Meyer
mesh_terms: D015104:3,4-Methylenedioxyamphetamine / Q000031:analogs & derivatives* / Q000032:analysis / Q000652:urine; D018759:Adrenergic Uptake Inhibitors / Q000032:analysis / Q000652:urine; D003042:Cocaine / Q000032:analysis / Q000652:urine*; D018765:Dopamine Uptake Inhibitors / Q000032:analysis / Q000652:urine; D004785:Environmental Pollutants / Q000032:analysis* / Q000652:urine; D006801:Humans; D013287:Illicit Drugs / Q000032:analysis / Q000652:urine*; D057230:Limit of Detection; D018817:N-Methyl-3,4-methylenedioxyamphetamine / Q000032:analysis / Q000652:urine*; D012987:Soil / Q000737:chemistry; D015813:Substance Abuse Detection / Q000379:methods*; D062065:Wastewater / Q000032:analysis*
chemical_list: D015104:3,4-Methylenedioxyamphetamine; D018759:Adrenergic Uptake Inhibitors; D003042:Cocaine; D018765:Dopamine Uptake Inhibitors; D004785:Environmental Pollutants; D013287:Illicit Drugs; D018817:N-Methyl-3,4-methylenedioxyamphetamine; D012987:Soil; D062065:Wastewater; C051800:3,4-methylenedioxyethamphetamine
keywords: illicit drugs; phase II metabolites; pooled urine analysis; stability; wastewater-based epidemiology