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Wastewater-based epidemiology is an additional indicator of drug use that is gaining reliability to complement the current established panel of indicators. The aims of this study were to: (i) assess spatial and temporal trends of population-normalized mass loads of benzoylecgonine, amphetamine, methamphetamine and 3,4-methylenedioxymethamphetamine (MDMA) in raw wastewater over 7 years (2011-17); (ii) address overall drug use by estimating the average number of combined doses consumed per day in each city; and (iii) compare these with existing prevalence and seizure data.Analysis of daily raw wastewater composite samples collected over 1 week per year from 2011 to 2017.Catchment areas of 143 wastewater treatment plants in 120 cities in 37 countries.Parent substances (amphetamine, methamphetamine and MDMA) and the metabolites of cocaine (benzoylecgonine) and of ΔBenzoylecgonine was the stimulant metabolite detected at higher loads in southern and western Europe, and amphetamine, MDMA and methamphetamine in East and North-Central Europe. In other continents, methamphetamine showed the highest levels in the United States and Australia and benzoylecgonine in South America. During the reporting period, benzoylecgonine loads increased in general across Europe, amphetamine and methamphetamine levels fluctuated and MDMA underwent an intermittent upsurge.The analysis of wastewater to quantify drug loads provides near real-time drug use estimates that globally correspond to prevalence and seizure data.

The analysis of illicit drugs in urban wastewater is the basis of wastewater-based epidemiology (WBE), and has received much scientific attention because the concentrations measured can be used as a new non-intrusive tool to provide evidence-based and real-time estimates of community-wide drug consumption. Moreover, WBE allows monitoring patterns and spatial and temporal trends of drug use. Although information and expertise from other disciplines is required to refine and effectively apply WBE, analytical chemistry is the fundamental driver in this field. The use of advanced analytical techniques, commonly based on combined chromatography-mass spectrometry, is mandatory because the very low analyte concentration and the complexity of samples (raw wastewater) make quantification and identification/confirmation of illicit drug biomarkers (IDBs) troublesome. We review the most-recent literature available (mostly from the last 5 years) on the determination of IDBs in wastewater with particular emphasis on the different analytical strategies applied. The predominance of liquid chromatography coupled to tandem mass spectrometry to quantify target IDBs and the essence to produce reliable and comparable results is illustrated. Accordingly, the importance to perform inter-laboratory exercises and the need to analyze appropriate quality controls in each sample sequence is highlighted. Other crucial steps in WBE, such as sample collection and sample pre-treatment, are briefly and carefully discussed. The article further focuses on the potential of high-resolution mass spectrometry. Different approaches for target and non-target analysis are discussed, and the interest to perform experiments under laboratory-controlled conditions, as a complementary tool to investigate related compounds (e.g., minor metabolites and/or transformation products in wastewater) is treated. The article ends up with the trends and future perspectives in this field from the authors' point of view. © 2016 Wiley Periodicals, Inc. Mass Spec Rev 37:258-280, 2018.

Introduction and Aims Wastewater analysis is a new approach developed to estimate illicit drug (ID) consumption in large communities, such as a city. We tested the ability of this approach to detect differences in consumption in different districts of a city. Design and Methods Consumption of cocaine, heroin, tetrahydrocannabinol (THC) (cannabis active principle), amphetamine, methamphetamine and ecstasy was estimated by analysis of selected drug excretion residues in composite 24 h samples of untreated urban wastewater by liquid chromatography–tandem mass spectrometry. Samples were collected from the inlet of the three main Milan wastewater treatment plants (WWTPs), each serving a district of the city (west, center and east). In each WWTP, samples were taken daily for seven consecutive days in November 2010 and March 2011. Results We observed significant differences of ID consumption (expressed as mg/day/1000 inhabitants) among districts: consumption of some ID was significantly higher in the eastern district (P

Residues of illicit drugs have been recently found in urban wastewater and surface water. Their levels reflect the amount of drugs collectively excreted by consumers and can therefore be used to estimate drug abuse. An overview of the most widely used illicit drugs and of the analytical methods used for their detection in wastewater and surface water is presented here. Solid-phase extraction and high performance liquid chromatography-tandem mass spectrometry are the techniques that have been used for these investigations. Instrumental conditions and fragmentation patterns of illicit drugs and their metabolites are described.

1. 8-epi-prostaglandin (PG) F2 alpha, a major F2 isoprostane, is produced in vivo by free radical-dependent peroxidation of lipid-esterified arachidonic acid. Both cyclo-oxygenase isoforms (COX-1 and COX-2) may also form free 8-epi-PGF2 alpha as a minor product. It has been recently seen in human volunteers that the overall basal formation of 8-epi-PGF2 alpha in vivo is mostly COX-independent and urinary 8-epi-PGF2 alpha is therefore an accurate marker of 'basal' oxidative stress in vivo. 2. To test the validity of this marker in the rat, we evaluated in vivo the effect of COX inhibition on the formation of 8-epi-PGF2 alpha vs prostanoids. Two structurally unrelated COX inhibitors (naproxen: 30 mg kg-1 day-1; indomethacin: 4 mg kg-1 day-1) were given i.p. to rats kept in metabolic cages. In vivo formation of 8-epi-PGF2 alpha was assessed by measuring its urinary excretion. Prostanoid biosynthesis was assessed by measuring urinary excretion of major metabolites of thromboxane (TX) and prostacyclin (2,3-dinor-TXB1 and 2,3-dinor-6-keto-PGF1 alpha). All compounds were selectively measured by immunopurification/gas chromatography-mass spectrometry. 3. Naproxen reduced urinary excretion of 2,3-dinor-TXB1 and 2,3-dinor-6-keto-PGF1 alpha but, unexpectedly, also that of 8-epi-PGF2 alpha (82, 49 and 52% inhibition, respectively). Indomethacin had a similar effect (77, 69 and 55% inhibition). Esterified 8-epi-PGF2 alpha in liver and plasma remained unchanged after indomethacin. 4. These findings prompted us to re-assess the contribution of COX activity to the systemic production of 8-epi-PGF2 alpha in man. We gave naproxen (1 g day-1) to healthy subjects (four nonsmokers and four smokers). Urinary 8-epi-PGF2 alpha remained unchanged in the two groups (9.63 +/- 0.99 before vs 10.24 +/- 1.01 after and 20.14 +/- 3.00 vs 19.03 +/- 2.45 ng h-1 1.73 m-2), whereas there was a marked reduction of major urinary metabolites of thromboxane and prostacyclin (about 90% for both 11-dehydro-TXB2 and 2,3-dinor-TXB2; > 50% for 2,3-dinor-6-keto-PGF1 alpha). 5. To investigate whether rat COX-1 produces 8-epi-PGF2 alpha more efficiently than human COX-1, we measured the ex vivo formation of 8-epi-PGF2 alpha and TXB2 simultaneously in whole clotting blood. Serum levels of 8-epi-PGF2 alpha and TXB2 were similar in rats and man. 6. We conclude that a significant amount of COX-dependent 8-epi-PGF2 alpha is present in rat but not in human urine under normal conditions. This implies that urinary 8-epi-PGF2 alpha cannot be used as an index of near-basal oxidant stress in rats. On the other hand, our data further confirm the validity of this marker in man.

PREFACE. CONTRIBUTORS. I INTRODUCTION. 1 ILLICIT DRUGS AND THE ENVIRONMENT (Christian G. Daughton). II THE PHYSIOLOGY OF ILLICIT DRUGS. 2 METABOLISM AND EXCRETION OF ILLICIT DRUGS IN HUMANS (Manuela Melis, Sara Castiglioni, and Ettore Zuccato). III MASS SPECTROMETRY IN ILLICIT DRUGS DETECTION AND MEASUREMENT CURRENT AND NOVEL ENVIRONMENTAL APPLICATIONS. 3 ANALYTICAL METHODS FOR THE DETECTION OF ILLICIT DRUGS IN WASTEWATERS AND SURFACE WATERS (Renzo Bagnati and Enrico Davoli). 4 WIDE-SCOPE SCREENING OF ILLICIT DRUGS IN URBAN WASTEWATER BY UHPLC-QTOF MS (Felix Hernadez, Juan V. Sancho, and Lubertus Bijlsma). 5 DETERMINATION OF ILLICIT DRUGS IN THE WATER CYCLE BY LC ORBITRAP MS (Pim de Voogt, Erik Emke, Rick Helmus, Pavlos Panteliadis, and Jan A. van Leerdam). IVA MASS SPECTROMETRIC ANALYSIS OF ILLICIT DRUGS IN THE ENVIRONMENT: OCCURRENCE AND FATE IN WASTEWATER AND SURFACE WATER. 6 OCCURRENCE OF ILLICIT DRUGS IN WASTEWATER IN SPAIN (Cristina Postigo, Miren Lopez de Alda, and Damia Barcelo). 7 OCCURRENCE OF ILLICIT DRUGS IN WASTEWATER AND SURFACE WATER IN ITALY (Sara Castiglioni and Ettore Zuccato). 8 OCCURRENCE OF ILLICIT DRUGS IN SURFACE WATER AND WASTEWATER IN THE UK (Barbara Kasprzyk-Hordern). 9 ON THE FRONTIER: ANALYTICAL CHEMISTRY AND THE OCCURRENCE OF ILLICIT DRUGS INTO SURFACE WATERS IN THE UNITED STATES (Tammy Jones-Lepp, David Alvarez, and Bommanna Loganathan). 10 MONITORING NONPRESCRIPTION DRUGS IN SURFACE WATER IN NEBRASKA (USA) (Shannon Bartelt-Hunt, and Daniel D. Snow). IVB MASS SPECTROMETRIC ANALYSIS OF ILLICIT DRUGS IN THE ENVIRONMENT: ILLICIT DRUGS IN DRINKING WATER. 11 PRESENCE AND REMOVAL OF ILLICIT DRUGS IN CONVENTIONAL DRINKING WATER TREATMENT PLANTS (Maria Huerta-Fontela, Maria Teresa Galceran, and Francesc Ventura). 12 ANALYSIS OF ILLICIT DRUGS IN WATER USING DIRECT-INJECTION LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY (Rebecca A. Trenholm and Shane A. Snyder). IVC MASS SPECTROMETRIC ANALYSIS OF ILLICIT DRUGS IN THE ENVIRONMENT: PRESENCE IN AIR AND SUSPENDED PARTICULATE MATTER. 13 PSYCHOTROPIC SUBSTANCES IN URBAN AIRBORNE PARTICULATES (Angelo Cecinato and Catia Balducci). V APPLICATIONS OF ILLICIT DRUG ANALYSIS IN THE ENVIRONMENT. 14 ILLICIT DRUGS IN THE ENVIRONMENT: IMPLICATION FOR ECOTOXICOLOGY (Guido Domingo, Kristin Schirmer, Marcella Bracale, and Francesco Pomati). 15 DRUG ADDICTION POTENTIAL OF A NEW APPROACH TO MONITORING DRUG CONSUMPTION (Norbert Frost). 16 ASSESSING ILLICIT DRUG CONSUMPTION BY WASTEWATER ANALYSIS: HISTORY, POTENTIAL, AND LIMITATION OF A NOVEL APPROACH (Ettore Zuccato and Sara Castiglioni). 17 COCAINE AND METABOLITES IN WASTEWATER AS A TOOL TO CALCULATE LOCAL AND NATIONAL COCAINE CONSUMPTION PREVALENCE IN BELGIUM (Alexander L.N. van Nuijs, Lieven Bervoets, Philippe G. Jorens, Ronny Blust, Hugo Neels, and Adrian Covaci). 18 MEASUREMENT OF ILLICIT DRUG CONSUMPTION IN SMALL POPULATIONS: PROGNOSIS FOR NONINVASIVE DRUG TESTING OF STUDENT POPULATIONS (Deepika Panawennage, Sara Castiglioni, Ettore Zuccato, Enrico Davoli, and M. Paul Chiarelli). VI CONCLUSIONS. 19 CONCLUSIONS AND FUTURE PERSPECTIVES (Roberto Fanelli). INDEX.

Lactose malabsorption, by the breath hydrogen test, and lactose intolerance (presence of symptoms) were studied in twenty healthy Italian subjects after intake of 12.5, 25 and 50 g lactose, whole milk and low-lactose milk. A rise in respiratory concentration of hydrogen (greater than 20 ppm) (malabsorption) was found in fifteen subjects after 50 g lactose, in thirteen after 25 g and in seven after 12.5 g. Symptoms generally occurred in subjects presenting a rise in respiratory hydrogen excretion, but such a rise was often observed without symptoms. Thirteen subjects presented symptoms after 50 g lactose, but only three after 25 g and one after 12.5 g. Whole milk (500 ml) gave a lower incidence of lactose malabsorption than 25 g lactose (7/20 versus 13/20, P less than 0.05) and more subjects developed symptoms (7/20 versus 3/20, NS). Low-lactose milk produced no malabsorbers and one intolerant. Breath methane was detected constantly in seven subjects and in three on some of the days of observation. Respiratory methane excretion generally appeared to be unrelated to lactose ingestion.