Structure confirmation, reactivity, bacterial mutagenicity and quantification of 2,2,4-tribromo-5-hydroxycyclopent-4-ene-1,3-dione in drinking water.

The presence of two new disinfectant by-product (DBP) groups in the UK was recently shown using non-target analysis, halogenated-hydroxycyclopentenediones and halogenated-methanesulfonic acids. In this work, we confirmed the structure of 2,2,4-tribromo-5-hydroxycyclopent-4-ene-1,3-dione (TBHCD), and quantified it together with dibromomethanesulfonic acid at 122 ± 34 and 326 ± 157 ng L on average in London's drinking water, respectively (n = 21). We found TBHCD to be photolabile and unstable in tap water and at alkaline pH.

Dog swimming and ectoparasiticide water contamination in urban conservation areas: A case study on Hampstead Heath, London.

Widespread occurrence of two ectoparasiticide compounds in the aquatic environment, imidacloprid and fipronil, have prompted concerns about their potential environmental impacts. However, very little focus has been placed on water bodies in urban green spaces used for dog swimming. In this study, occurrence of both substances on Hampstead Heath, London, was compared in ponds with (n = 3) and without dog swimming activity (n = 3), as well as connecting streams above, between, and below these ponds (n = 6).

Pollution of Soil by Pharmaceuticals: Implications for Metazoan and Environmental Health.

The use of pharmaceuticals has grown substantially and their consequential release via wastewaters poses a potential threat to aquatic and terrestrial environments. While transportation prediction models for aquatic environments are well established, they cannot be universally extrapolated to terrestrial systems. Pharmaceuticals and their metabolites are, for example, readily detected in the excreta of terrestrial organisms (including humans).

Exploring the Chemical Space of the Exposome: How Far Have We Gone?

Around two-thirds of chronic human disease can not be explained by genetics alone. The Lancet Commission on Pollution and Health estimates that 16% of global premature deaths are linked to pollution. Additionally, it is now thought that humankind has surpassed the safe planetary operating space for introducing human-made chemicals into the Earth System.

Exploring the chemical subspace of RPLC: A data driven approach.

Background: The chemical space is comprised of a vast number of possible structures, of which an unknown portion comprises the human and environmental exposome. Such samples are frequently analyzed using non-targeted analysis via liquid chromatography (LC) coupled to high-resolution mass spectrometry often employing a reversed phase (RP) column. However, prior to analysis, the contents of these samples are unknown and could be comprised of thousands of known and unknown chemical constituents.

Apportioning sources of chemicals of emerging concern along an urban river with inverse modelling.

Concentrations of chemicals in river water provide crucial information for assessing environmental exposure and risks from fertilisers, pesticides, heavy metals, illicit drugs, pathogens, pharmaceuticals, plastics and perfluorinated substances, among others. However, using concentrations measured along waterways (e.g.

Down-the-drain pathways for fipronil and imidacloprid applied as spot-on parasiticides to dogs: Estimating aquatic pollution.

Fipronil and imidacloprid have been widely detected in UK surface waters in recent years, often at concentrations that ecotoxicological studies have shown can harm aquatic life. Down-the-drain (DTD) passage of pet flea and tick treatments are being implicated as an important source, with many of the UK's 22 million cats and dogs receiving routine, year-round preventative doses containing these parasiticides. The UK Water Industry's 3rd Chemical Investigation Programme (UKWIR CIP3) has confirmed wastewater as a major entry pathway for these chemicals into surface waters, but the routes by which they enter the wastewater system remain unclear.

A One-Health environmental risk assessment of contaminants of emerging concern in London's waterways throughout the SARS-CoV-2 pandemic.

The SARS-CoV-2 pandemic had huge impacts on global urban populations, activity and health, yet little is known about attendant consequences for urban river ecosystems. We detected significant changes in occurrence and risks from contaminants of emerging concern (CECs) in waterways across Greater London (UK) during the pandemic. We were able to rapidly identify and monitor large numbers of CECs in n = 390 samples across 2019-2021 using novel direct-injection liquid chromatography-mass spectrometry methods for scalable targeted analysis, suspect screening and prioritisation of CEC risks.

International Comparison, Risk Assessment, and Prioritisation of 26 Endocrine Disrupting Compounds in Three European River Catchments in the UK, Ireland, and Spain.

Endocrine-disrupting compounds (EDCs) constitute a wide variety of chemistries with diverse properties that may/can pose risks to both humans and the environment. Herein, a total of 26 compounds, including steroids, flame retardants, and plasticizers, were monitored in three major and heavily urbanized river catchments: the R. Liffey (Ireland), the R.

Enhanced selectivity for acidic contaminants in drinking water: From suspect screening to toxicity prediction.

A novel analytical workflow for suspect screening of organic acidic contaminants in drinking water is presented, featuring selective extraction by silica-based strong anion-exchange solid-phase extraction, mixed-mode liquid chromatography-high resolution accurate mass spectrometry (LC-HRMS), peak detection, feature reduction and compound identification. The novel use of an ammonium bicarbonate-based elution solvent extended strong anion-exchange solid-phase extraction applicability to LC-HRMS of strong acids. This approach performed with consistently higher recovery and repeatability (88 ± 7 % at 500 ng L), improved selectivity and lower matrix interference (mean = 12 %) over a generic mixed-mode weak anion exchange SPE method.

A year-long study of the occurrence and risk of over 140 contaminants of emerging concern in wastewater influent, effluent and receiving waters in the Republic of Ireland.

Despite being a developed country in the European Union (EU), knowledge of the nature and extent of contamination of water bodies with contaminants of emerging concern (CECs) in Ireland is limited. In this study, >140 CECs including pharmaceuticals, pesticides and personal care products were monitored in monthly samples of wastewater treatment plant (WWTP) influent, effluent and receiving surface waters at both an urban and a rural location (72 samples in total) in Ireland over a 12-month period in 2018-2019. In total, 58 CECs were detected, including several EU Water Framework Directive Watch List compounds.

Occurrence of Z-drugs, benzodiazepines, and ketamine in wastewater in the United States and Mexico during the Covid-19 pandemic.

Z-drugs, benzodiazepines and ketamine are classes of psychotropic drugs prescribed for treating anxiety, sleep disorders and depression with known side effects including an elevated risk of addiction and substance misuse. These drugs have a strong potential for misuse, which has escalated over the years and was hypothesized here to have been exacerbated during the COVID-19 pandemic. Wastewater-based epidemiology (WBE) constitutes a fast, easy, and relatively inexpensive approach to epidemiological surveys for understanding the incidence and frequency of uses of these drugs.

A miniaturized passive sampling-based workflow for monitoring chemicals of emerging concern in water.

The miniaturization of a full workflow for identification and monitoring of contaminants of emerging concern (CECs) is presented. Firstly, successful development of a low-cost small 3D-printed passive sampler device (3D-PSD), based on a two-piece methacrylate housing that held up to five separate 9 mm disk sorbents, is discussed. Secondly, a highly sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method reduced the need for large scale in-laboratory apparatus, solvent, reagents and reference material quantities for in-laboratory passive sampler device (PSD) calibration and extraction.

Quantitative Determination and Environmental Risk Assessment of 102 Chemicals of Emerging Concern in Wastewater-Impacted Rivers Using Rapid Direct-Injection Liquid Chromatography-Tandem Mass Spectrometry.

The rapid source identification and environmental risk assessment (ERA) of hundreds of chemicals of emerging concern (CECs) in river water represent a significant analytical challenge. Herein, a potential solution involving a rapid direct-injection liquid chromatography-tandem mass spectrometry method for the quantitative determination of 102 CECs (151 qualitatively) in river water is presented and applied across six rivers in Germany and Switzerland at high spatial resolution. The method required an injection volume of only 10 µL of filtered sample, with a runtime of 5.

The transportation, transformation and (bio)accumulation of pharmaceuticals in the terrestrial ecosystem.

Soil dwelling organisms, plants and many primary consumers in food webs face the challenge of exposure to contaminants of emerging concern (CECs) present in terrestrial systems, including thousands of substances derived from pharmaceutical and personal care products (PPCPs). The recent increase in the consumption of modern human or veterinary drugs has resulted in a surge of anthropogenic pharmaceuticals, frequently introduced into terrestrial environments via untreated/treated wastewater. Pharmaceuticals display diverse degradation and accumulation behaviours in receiving bodies, however their impact on soils has, at large, been overlooked.

Rapid direct analysis of river water and machine learning assisted suspect screening of emerging contaminants in passive sampler extracts.

A novel and rapid approach to characterise the occurrence of contaminants of emerging concern (CECs) in river water is presented using multi-residue targeted analysis and machine learning-assisted in silico suspect screening of passive sampler extracts. Passive samplers (Chemcatcher®) configured with hydrophilic-lipophilic balanced (HLB) sorbents were deployed in the Central London region of the tidal River Thames (UK) catchment in winter and summer campaigns in 2018 and 2019. Extracts were analysed by; (a) a rapid 5.

Perchlorate detection an invertebrate biosensor.

Improvised explosive devices (IEDs) are constructed from easily obtainable ingredients that are often unregulated and difficult to trace. Salts of the oxyhalide perchlorate are frequently used as oxidisers in IEDs and in commercially available munitions, thus a reliable detection is needed to aid forensic investigations and the tracing of environmental ground or surface water contamination. We introduce the nematode Caenorhabditis elegans as a biosensor for the presence of perchlorate, a promising alternative to the costly, technically challenging and time-consuming current perchlorate detection methods.

Quantitative Assessment of Dietary (Poly)phenol Intake: A High-Throughput Targeted Metabolomics Method for Blood and Urine Samples.

Many studies have associated the consumption of (poly)phenol-rich diets with health benefits. However, accurate high-throughput quantitative methods for estimating exposure covering a broad spectrum of (poly)phenols are lacking. We have developed and validated a high-throughput method for the simultaneous quantification of 119 (poly)phenol metabolites in plasma and urine using ultra high-performance liquid chromatography coupled with triple quadrupole mass spectrometry, with a very fast sample treatment and a single run time of 16 min.

Multicompartment and cross-species monitoring of contaminants of emerging concern in an estuarine habitat.

The fate of many chemicals in the environment, particularly contaminants of emerging concern (CEC), have been characterised to a limited extent with a major focus on occurrence in water. This study presents the characterisation, distribution and fate of multiple chemicals including pharmaceuticals, recreational drugs and pesticides in surface water, sediment and fauna representing different food web endpoints in a typical UK estuary (River Colne, Essex, UK). A comparison of contaminant occurrence across different benthic macroinvertebrates was made at three sites and included two amphipods (Gammarus pulex &Crangon crangon), a polychaete worm (Hediste diversicolor) and a gastropod (Peringia ulvae).

Trace multi-class organic explosives analysis in complex matrices enabled using LEGO®-inspired clickable 3D-printed solid phase extraction block arrays.

The development of a new, lower cost method for trace explosives recovery from complex samples is presented using miniaturised, click-together and leak-free 3D-printed solid phase extraction (SPE) blocks. For the first time, a large selection of ten commercially available 3D printing materials were comprehensively evaluated for practical, flexible and multiplexed SPE using stereolithography (SLA), PolyJet and fused deposition modelling (FDM) technologies. Miniaturised single-piece, connectable and leak-free block housings inspired by Lego® were 3D-printed in a methacrylate-based resin, which was found to be most stable under different aqueous/organic solvent and pH conditions, using a cost-effective benchtop SLA printer.

High-throughput multi-residue quantification of contaminants of emerging concern in wastewaters enabled using direct injection liquid chromatography-tandem mass spectrometry.

A rapid quantitative method for 135 contaminants of emerging concern (CECs) in untreated wastewater enabled with direct injection liquid chromatography-tandem mass spectrometry is presented. All compounds were analysed within 5 min on a short biphenyl cartridge using only 10 μL of filtered sample per injection. Up to 76 compounds were monitored simultaneously during the gradient (including mostly two transitions per compound and stable isotope-labelled analogues) while yielding >10 data points per peak.

Untargeted metabolomics changes on Gammarus pulex induced by propranolol, triclosan, and nimesulide pharmaceutical drugs.

The presence of pharmaceuticals and personal care products (PPCPs) in natural water resources due to incomplete removal in Wastewater Treatment Plants (WWTPs) is a serious environmental concern at present. In this work, the effects of three pharmaceuticals (propranolol, triclosan, and nimesulide) on Gammarus pulex metabolic profiles at different doses and times of exposure have been investigated by liquid chromatography coupled to high-resolution mass spectrometry (LC-HRMS). The complex data sets generated in the different exposure experiments were analyzed with the ROIMCR procedure, based on the selection of the MS regions of interest (ROI) data and on their analysis by the Multivariate Curve-Resolution Alternating Least Squares (MCR-ALS) chemometrics method.

Spatio-temporal assessment of illicit drug use at large scale: evidence from 7 years of international wastewater monitoring.

Background And Aims: 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.

Design: Analysis of daily raw wastewater composite samples collected over 1 week per year from 2011 to 2017.

Improved determination of femtogram-level organic explosives in multiple matrices using dual-sorbent solid phase extraction and liquid chromatography-high resolution accurate mass spectrometry.

Identification and trace quantification of multiple explosives residues, their precursors and transformation products in complex samples remains very challenging. For solid phase extraction (SPE) and liquid chromatography-high resolution accurate mass spectrometry-based methods (LC-HRMS), interferences from co-extracted matrix components can significantly affect recovery during extraction and/or detector signal. The aim of this work was to develop a new, improved and more generalisable extraction approach to trace explosives analysis in a range of matrices using dual-sorbent SPE with LC-HRMS.