Analysis of drugs of abuse by online SPE-LC high resolution mass spectrometry: Communal assessment of consumption Nubia V. Heuett a,b , Cesar E. Ramirez a,b , Adolfo Fernandez b , Piero R. Gardinali a,b, ⁎ a Department of Chemistry and Biochemistry, Florida International University, North Miami, FL 33181, USA b Southeast Environmental Research Center, Florida International University, Miami, FL 33199, USA HIGHLIGHTS • Online-SPE-LC–HRMS analysis of 18 illicit drugs and metabolites in sewage influents • Positive detection of 14 drugs of abuse and metabolites in a college campus setting • Consumption estimates were determined for amphetamine, THC, cocaine, and heroin. abstract article info Article history: Received 9 October 2014 Received in revised form 16 December 2014 Accepted 16 December 2014 Available online xxxx Editor: D. Barcelo Keywords: Illicit drugs Online-SPE High resolution mass spectrometry College campus Sewage influents An online SPE-LC–HRMS method was developed to monitor the consumption of 18 drugs of abuse (DOAs) in- cluding amphetamines, opioids, cocainics, cannabinoids, lysergics, and their corresponding metabolites in a well characterized college campus setting via wastewater analysis. Filtered and diluted (10×) sewage water sam- ples (5 mL inj.) were automatically pre-concentrated and analyzed in 15 min using a Thermo EQuan MAX online SPE system equipped with a HyperSep™ Retain PEP (20 × 2.1 mm × 12 μm) SPE column and a Hypersil Gold™ aQ (150 × 2.1 mm × 3 μm) analytical column. A Q Exactive™ Hybrid Quadrupole-Orbitrap HRMS was used in full scan mode (R = 140,000) for positive identification, and quantitation of target compounds. Method detection limits for all analytes ranged between 0.6 and 1.7 ng/L in sewage. A total of 14 DOAs were detected from two dif- ferent locations (dorms and main college campus) within a one-year period. Most frequently detected drugs throughout the entire study were amphetamine (N 96%) and THC's metabolite 11-nor-9-carboxy-Δ-9-THC (N 100%) with maximum concentrations of 5956 and 2413 ng/L respectively. Daily doses per 1000 people were determined in order to assess consumption of THC, amphetamine, heroin and cocaine, in both dorms and main campus. © 2014 Elsevier B.V. All rights reserved. 1. Introduction Every year, the United Nations Office on Drugs and Crime (UNODC) generates a comprehensive report on the latest developments in drug markets, covering production, trafficking, consumption, and health con- sequences (UNODC, 2014). In the year 2012, the US alone reached its highest levels of illicit drug use in the past 10 years (16% of the popula- tion 12 years and older), with consumption being the greatest among those in their late teens or early twenties, as noted in the World Drug Report 2014 (UNODC, 2014). These figures, however, are not evaluated fast enough to provide real time understanding of the situation for law enforcement officials to take appropriate timely actions. Multiple studies have reported wastewater-derived figures for the consumption of drugs of abuse (illicit and prescription drugs), as they provide a nonintrusive way to quickly assess social trends, usage patterns, and drug prevalence at the community level (Castiglioni et al., 2006; Zuccato et al., 2008; Chiaia and Banta-green, 2008; Huerta-Fontela et al., 2008; Bartelt-hunt et al., 2009; Boleda et al., 2009; Postigo et al., 2010; Baker and Kasprzyk-hordern, 2011; Nuijs et al., 2011; Bijlsma et al., 2012; Kasprzyk-Hordern and Baker, 2012). This in contrast to the more conservative, time-consuming, and intrusive approaches of social surveys, drug seizures, crime statistics, and medical examiner reports (Nuijs et al., 2009d; Baker and Kasprzyk-hordern, 2011; Burgard et al., 2013). Besides the social, health, and economic implications illicit drugs pose, there is also the impact that these drugs could inflict over aquatic environ- ments. For instance, Parolini et al. reported that exposure to 0.5 μg/L and 1 μg/L of cocaine (benzoylecgonine) caused oxidative stress in freshwater bivalve Dreissena polymorpha, due to imbalances of the enzyme defense chain (Parolini et al., 2013). Similarly to pharmaceuticals, illicit drugs are metabolized in the body and excreted in their unchanged form or as Science of the Total Environment 511 (2015) 319–330 ⁎ Corresponding author at: 3000 NE 151st ST, FIU Biscayne Bay Campus, MSB-350, North Miami, FL 33181, USA. E-mail addresses: nheuett@fiu.edu (N.V. Heuett), cramirez@fiu.edu (C.E. Ramirez), amfernan@fiu.edu (A. Fernandez), gardinal@fiu.edu (P.R. Gardinali). http://dx.doi.org/10.1016/j.scitotenv.2014.12.043 0048-9697/© 2014 Elsevier B.V. All rights reserved. Contents lists available at ScienceDirect Science of the Total Environment journal homepage: www.elsevier.com/locate/scitotenv