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Background and Aims Design, setting, participants, measurements Findings Conclusions Between 2018 and 2020, Australia implemented major policy changes to improve the quality and safety of opioid prescribing, with a specific focus on oxycodone. This study used wastewater‐based epidemiology to assess the efficacy of Australia's regulatory reforms by measuring change in consumption of oxycodone via exploratory analysis.Wastewater analysis data on oxycodone consumption was from the National Wastewater Drug Monitoring Program. The program captures data from more than 50 wastewater treatment plant catchments across Australia, equivalent to more than 50% of the national population. Geographic trend analyses were conducted for both major cities and regional areas within all states and territories of Australia over a 6‐year period between 2017 and 2023.Oxycodone consumption showed a statistically significant increase nationally from 78 mg/day/1000 people (95% confidence interval [CI] = 71, 84) in 2017 to 120 mg/day/1000 people in August 2019 (95% CI = 110, 120), an increase of 52% (95% CI = 42, 62, P < 0.0001). From August 2019 to December 2020, there was a statistically significant decrease from 120 to 65 mg/day/1000 people (95% CI = 60, 71), a decrease of 45% (95% CI = 40, 51), followed by a modest 2.4% increase to the end of the study period in April 2023 (95% CI [2.0,2.7]).A 45% reduction in oxycodone consumption in Australia from 2019 to 2020 coincided with national policy changes that aimed to reduce consumption of prescription opioids. The overall declining trend in consumption was suggestive of the effectiveness of national interventions in reducing pharmaceutical opioid use. Wastewater‐based epidemiology provides an effective approach for assessing the effectiveness of controlled substances policy changes. [ABSTRACT FROM AUTHOR]

This research explored the potential of marble wastewater (MWW) in cement paste and mortar production, addressing water scarcity, sustainable growth, and resource management. It investigated the physico-mechanical properties and microstructure of cement materials incorporated with varying amounts of MWW. In this study, we utilized tap water and MWW for mortar quality testing, focusing on parameters including setting times, water absorption, and mechanical strength. The viability of MWW in concrete formulations was confirmed by its acceptable total dissolved solids and alkalinity levels. A comprehensive experimental program determined that using marble wastewater in place of tap water reduced the quantity of water required for cement consistency and generated slightly higher compressive strengths (2, 3, 4, and 6%) after 28 days of curing. Analytical techniques, including Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), energy-dispersive X-ray analysis, and X-ray diffraction (XRD), were employed for molecular and microstructural analyses, which revealed that MWW had a significant influence on portlandite development and CSH formation at higher replacement levels. In short, this research highlights the feasibility of using MWW in cement products, contributing to sustainable water resources, and industrial waste management and utilization. [ABSTRACT FROM AUTHOR]

The development of low-cost and highly sensitive ratiometric fluorescence sensor, CdTe@MIPs/MgF2, for N-Ethylpentylone (NEP) detection in wastewater samples is described. In this system, CdTe@MIPs (λex = 370, λem = 570) are employed as the receptor and response unit for NEP, with MgF2 (λex = 370, λem = 470) as the reference signal to enhance stability. Under optimal conditions, the sensor shows fluorescent quenching response at 570 nm to NEP in linear range of 2–200 nM, with LOD of 0.6 nM. The sensor also demonstrates significant selectivity for NEP over other analogues and interferents, making it ideal for practical applications in wastewater analysis. This approach is potentially more cost-effective and sensitive than conventional mass spectrometry in detecting abused substances in sewage. Additionally, the MgF2 fluorescent nano-material was first-ever developed and investigated, which may be significant in future research. [ABSTRACT FROM AUTHOR]

Abstract In this research, a novel magnetic zirconium-based metal-organic framework (Fe3O4@SiO2@MIP-202, MMOF), was fabricated, fully characterized, and applied for the batch-mode solid phase extraction of trace amounts of Pd2+ ions from water and wastewater samples before its spectrophotometric detection. Pd2+ ions were desorbed from MMOF by nitric acid and were complexed by treating with KI solution to have a maximum absorbance at 410 nm. The synthesized MMOF composite showed a very large surface area (65 m2.g− 1), good magnetization (1.7 emu.g− 1) and a large pore volume (0.059 cm3.g− 1) with adsorption capacity of 194.5 mg of Pd2+ ions/g of the adsorbent. This nanosorbent boasts chemo-mechanical stability, high adsorption capacity due to its vast active sites, and facile recovery facilitated by its magnetic properties. Parameters affecting the extraction efficiency of the method were optimized as pH of the sample 7.4, volume of the sample 25 mL, 15 mg adsorbent, 1 mL of 0.1 M HNO3 eluent, with 10 and 15 min as the extraction and desorption times, respectively. The calibration curve was found to be linear across the 10.0–1500.0 µg.L− 1 range with a limit of detection of 1.05 µg.L− 1. The obtained extraction efficiency and enrichment were 98% and 245, respectively. The total analysis time was less than 30 min. This MMOF has never been used for the extraction of Pd2+ ions before.

In this research, a novel magnetic zirconium-based metal-organic framework (Fe3O4@SiO2@MIP-202, MMOF), was fabricated, fully characterized, and applied for the batch-mode solid phase extraction of trace amounts of Pd2+ ions from water and wastewater samples before its spectrophotometric detection. Pd2+ ions were desorbed from MMOF by nitric acid and were complexed by treating with KI solution to have a maximum absorbance at 410 nm. The synthesized MMOF composite showed a very large surface area (65 m2.g− 1), good magnetization (1.7 emu.g− 1) and a large pore volume (0.059 cm3.g− 1) with adsorption capacity of 194.5 mg of Pd2+ ions/g of the adsorbent. This nanosorbent boasts chemo-mechanical stability, high adsorption capacity due to its vast active sites, and facile recovery facilitated by its magnetic properties. Parameters affecting the extraction efficiency of the method were optimized as pH of the sample 7.4, volume of the sample 25 mL, 15 mg adsorbent, 1 mL of 0.1 M HNO3 eluent, with 10 and 15 min as the extraction and desorption times, respectively. The calibration curve was found to be linear across the 10.0–1500.0 µg.L− 1 range with a limit of detection of 1.05 µg.L− 1. The obtained extraction efficiency and enrichment were 98% and 245, respectively. The total analysis time was less than 30 min. This MMOF has never been used for the extraction of Pd2+ ions before. [ABSTRACT FROM AUTHOR]

In this work, the development of a novel method for the detection of mercury (II) ions in wastewater using a mercury ion-imprinted polymer (IIP) combined with a quartz crystal microbalance (QCM) is described. The IIP was successfully synthesized via the polymerization of a of a novel fluorescein- and 2-aminophenol-functionalized methacrylic acid monomer, which was noted to have high binding affinity to mercury (II) ions. This polymer was subsequently coated on a QCM chip to create an IIP-QCM sensor. This sensor was established to have high selectivity and good sensitivity to mercury (II) ions, and had a limit of detection (LOD) of 14.17 ppb, a limit of quantification (LOQ) of 42.94 ppb, a signal-to-noise ratio (S/N) of 4.29, good repeatability, and a working range of 42.94 ppb to 2 ppm. The sensor was also able to analyze tap water and wastewater samples. The IIP-QCM is, therefore, promising as a highly selective, cost-effective, and rapid mercury ion sensor for applications involving the detection of mercury in wastewater. [ABSTRACT FROM AUTHOR]

Wastewater-based epidemiology (WBE) is a robust tool for disease surveillance and monitoring of pharmaceutical consumption. However, monitoring tuberculosis (TB) drug consumption faces challenges due to limited data availability. This study aimed to optimise methods for detecting TB drugs in treated and untreated wastewater from four African countries: South Africa, Nigeria, Kenya, and Cameroon. The limit of detection (LOD) for these drugs ranged from a minimum of 2.20 (±1.02) for rifampicin to a maximum of 2.95 (±0.79) for pyrazinamide. A parallel trend was observed concerning the limit of quantification (LOQ), with rifampicin reporting the lowest average LOQ of 7.33 (±3.44) and pyrazinamide showing the highest average LOQ of 9.81 (±2.64). The variance in LOD and LOQ values could be attributed to factors such as drug polarity. Erythromycin and rifampicin exhibited moderately polar LogP values (2.6 and 2.95), indicating higher lipid affinity and lower water affinity.Conversely, ethambutol, pyrazinamide, and isoniazid displayed polar LogP values (−0.059, −0.6, and −0.7), suggesting lower lipid affinity and greater water affinity. The study revealed that storing wastewater samples for up to 5 days did not result in significant drug concentration loss, with concentration reduction remaining below 1 log throughout the storage period. Application of the optimised method for drug detection and quantification in both treated and untreated wastewater unveiled varied results. Detection frequencies varied among drugs, with ethambutol consistently most detected, while pyrazinamide and isoniazid were least detected in wastewater from only two countries. Most untreated wastewater samples had undetectable drug concentrations, ranging from 1.21 ng/mL for erythromycin to 54.61 ng/mL for isoniazid. This variability may suggest differences in drug consumption within connected communities. In treated wastewater samples, detectable drug concentrations ranged from 1.27 ng/mL for isoniazid to 10.20 ng/mL for ethambutol. Wastewater treatment plants exhibited variable removal efficiencies for different drugs, emphasising the need for further optimisation. Detecting these drugs in treated wastewater suggests potential surface water contamination and subsequent risks of human exposure, underscoring continued research's importance.

This research explored the potential of marble wastewater (MWW) in cement paste and mortar production, addressing water scarcity, sustainable growth, and resource management. It investigated the physico-mechanical properties and microstructure of cement materials incorporated with varying amounts of MWW. In this study, we utilized tap water and MWW for mortar quality testing, focusing on parameters including setting times, water absorption, and mechanical strength. The viability of MWW in concrete formulations was confirmed by its acceptable total dissolved solids and alkalinity levels. A comprehensive experimental program determined that using marble wastewater in place of tap water reduced the quantity of water required for cement consistency and generated slightly higher compressive strengths (2, 3, 4, and 6%) after 28 days of curing. Analytical techniques, including Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), energy-dispersive X-ray analysis, and X-ray diffraction (XRD), were employed for molecular and microstructural analyses, which revealed that MWW had a significant influence on portlandite development and CSH formation at higher replacement levels. In short, this research highlights the feasibility of using MWW in cement products, contributing to sustainable water resources, and industrial waste management and utilization.

An automated microextraction by packed sorbent followed by liquid chromatography–tandem mass spectrometry (MEPS-LC–MS/MS) method was developed for the determination of four endocrine disruptors—parabens, benzophenones, and synthetic phenolic antioxidants—in wastewater samples. The method utilizes a lab-made repackable MEPS device and a multi-syringe robotic platform that provides flexibility to test small quantities (2 mg) of multiple extraction phases and enables high-throughput capabilities for efficient method development. The overall performance of the MEPS procedure, including the investigation of influencing variables and the optimization of operational parameters for the robotic platform, was comprehensively studied through univariate and multivariate experiments. Under optimized conditions, the target analytes were effectively extracted from a small sample volume of 1.5 mL, with competitive detectability and analytical confidence. The limits of detection ranged from 0.15 to 0.30 ng L−1, and the intra-day and inter-day relative standard deviations were between 3 and 21%. The method's applicability was successfully demonstrated by determining methylparaben, propylparaben, butylated hydroxyanisole, and oxybenzone in wastewater samples collected from the São Carlos (SP, Brazil) river. Overall, the developed method proved to be a fast, sensitive, reliable, and environmentally friendly analytical tool for water quality monitoring. [ABSTRACT FROM AUTHOR]

This paper aims to provide an overview of the contemporary quantitative methods to assess alcohol consumption. We identified and rated six data collection methods according to four typical aims (i.e. to assess: per capita consumption, drinking patterns, event-specific consumption, and consumption over time) and five desirable features (low cognitive bias, contextual information, low participant and researcher burden, low costs). The results are presented in an overview table, which reveals that questionnaire-based methods are easy and cost-efficient but often distorted by cognitive biases. These biases can be avoided by analyzing sales/production statistics and wastewater samples, but these methods are unable to provide information on individual drinking patterns. Breathalyzers or transdermal monitors enable relatively precise measurement of individual consumption without any cognitive bias. However, the required devices are expensive and difficult to apply correctly, which makes data collection time, labor, and cost-intensive, particularly as sample sizes increase. Ecological momentary assessment (e.g. series of questionnaires within short timeframes completed in the participants' natural environments) reduces, but does not eliminate, cognitive biases and maximizes ecological validity. Unfortunately, this method also increases the response burden, potentially resulting in assessment reactivity and drop-out. Highlighting the combination of strengths and weaknesses of each method, this overview may serve as useful guidance for study planning and implementation. [ABSTRACT FROM AUTHOR]

In this work, the development of a novel method for the detection of mercury (II) ions in wastewater using a mercury ion-imprinted polymer (IIP) combined with a quartz crystal microbalance (QCM) is described. The IIP was successfully synthesized via the polymerization of a of a novel fluorescein- and 2-aminophenol-functionalized methacrylic acid monomer, which was noted to have high binding affinity to mercury (II) ions. This polymer was subsequently coated on a QCM chip to create an IIP-QCM sensor. This sensor was established to have high selectivity and good sensitivity to mercury (II) ions, and had a limit of detection (LOD) of 14.17 ppb, a limit of quantification (LOQ) of 42.94 ppb, a signal-to-noise ratio (S/N) of 4.29, good repeatability, and a working range of 42.94 ppb to 2 ppm. The sensor was also able to analyze tap water and wastewater samples. The IIP-QCM is, therefore, promising as a highly selective, cost-effective, and rapid mercury ion sensor for applications involving the detection of mercury in wastewater.

This work presents the synthesis and modification of cost-effective groundnut shell-based carbon sorbent and its utilization to extract chlorinated hydrocarbons from wastewater. The synthesized carbon sorbent was doped with nitrogen by treatment with melamine and further decorated with different weight percent of nickel by solid-state impregnation to achieve nickel-decorated nitrogen-doped carbon sorbents. The physicochemical properties of the sorbents were studied using Brunauer–Emmett–Teller, Fourier transform infrared spectroscopy, and field-emission scanning electron microscope. Each sorbent was then sealed into a polypropylene membrane like a tea bag and utilized to extract the chlorinated hydrocarbons from an aqueous sample and quantified using GC–MS. All the extraction-related parameters were optimized. The overall process presented a wide linear range (10–800 ng mL−1) with a coefficient of correlation between 0.9875 and 0.9943. The limit of detection (1.85–3.45 ng mL−1) and reproducibility (1.2–11%) were observed with relative recovery from the wastewater sample in the range of 85.4 to 114%. [ABSTRACT FROM AUTHOR]

Abstract Background The genomes of SARS-CoV-2 are classified into variants, some of which are monitored as variants of concern (e.g. the Delta variant B.1.617.2 or Omicron variant B.1.1.529). Proportions of these variants circulating in a human population are typically estimated by large-scale sequencing of individual patient samples. Sequencing a mixture of SARS-CoV-2 RNA molecules from wastewater provides a cost-effective alternative, but requires methods for estimating variant proportions in a mixed sample. Results We propose a new method based on a probabilistic model of sequencing reads, capturing sequence diversity present within individual variants, as well as sequencing errors. The algorithm is implemented in an open source Python program called VirPool. We evaluate the accuracy of VirPool on several simulated and real sequencing data sets from both Illumina and nanopore sequencing platforms, including wastewater samples from Austria and France monitoring the onset of the Alpha variant. Conclusions VirPool is a versatile tool for wastewater and other mixed-sample analysis that can handle both short- and long-read sequencing data. Our approach does not require pre-selection of characteristic mutations for variant profiles, it is able to use the entire length of reads instead of just the most informative positions, and can also capture haplotype dependencies within a single read.

Background and aim: From 1 February 2018, codeine was rescheduled from an over‐the‐counter (OTC) to a prescription‐only medicine in Australia. We used wastewater‐based epidemiology to measure changes in population codeine consumption before and after rescheduling. Methods: We analysed 3703 wastewater samples from 48 wastewater treatment plants, taken between August 2016 and August 2019. Our samples represented 10.6 million people, 45% of the Australian population in state capitals and regional areas in each state or territory. Codeine concentrations were determined by liquid chromatography–tandem mass spectrometry and converted to per‐capita consumption estimates using the site daily wastewater volume, catchment populations and codeine excretion kinetics. Results: Average per‐capita consumption of codeine decreased by 37% nationally immediately after the rescheduling in February 2018 [95% confidence interval (CI) = 35.3–39.4%] and substantially in all states between 24 and 51% (95% CI = 22.4–27.0% and 41.8–59.4%). The decrease was sustained at the lower level to August 2019. Locations with least pharmacy access decreased by 51% (95% CI = 41.7–61.7%), a greater decrease than 37% observed for those with greater pharmacy access (95% CI = 35.1–39.4%). Regional areas decreased by a smaller margin to cities (32 versus 38%, 95% CI = 30.2–34.1% versus 34.9–40.4%, respectively) from a base per‐capita usage approximately 40% higher than cities. Conclusion: Wastewater analysis shows that codeine consumption in Australia decreased by approximately 37% following its rescheduling as a prescription‐only medicine in 2018. Wastewater‐based epidemiology can be used to evaluate changes in population pharmaceutical consumption in responses to changes in drug scheduling. [ABSTRACT FROM AUTHOR]

The paper presents the validation of an electrochemical procedure for on-site Hg2+ ions determination in wastewater samples using a modified carbon screen-printed electrode (SPE) with a complexing polymeric film based on poly(2,2′-(ethane-1,2-diylbis((2-(azulen-2-ylamino)-2-oxoethyl)azanediyl))diacetic acid) (polyL). Using metal ions accumulation in an open circuit followed by anodic stripping voltammetry, the SPE-polyL electrode presents a linear range in the range of 20 µg/L to 150 µg/L, with a limit of detection (LOD) = 6 µg/L, limit of quantification (LOQ) = 20 µg/L, and an average measurement uncertainty of 26% of mercury ions. The results obtained in situ and in the laboratory using the SPE-polyL modified electrode were compared with those obtained by the atomic absorption spectrometry coupled with the cold vapor generation standardized method, with the average values indicating excellent recovery yields. [ABSTRACT FROM AUTHOR]

The proliferation of new psychoactive substances (NPS) over recent years has made their surveillance complex. The analysis of raw municipal influent wastewater can allow a broader insight into community consumption patterns of NPS. This study examines data from an international wastewater surveillance program that collected and analysed influent wastewater samples from up to 47 sites in 16 countries between 2019 and 2022. Influent wastewater samples were collected over the New Year period and analysed using validated liquid chromatography – mass spectrometry methods. Over the three years, a total of 18 NPS were found in at least one site. Synthetic cathinones were the most found class followed by phenethylamines and designer benzodiazepines. Furthermore, two ketamine analogues, one plant based NPS (mitragynine) and methiopropamine were also quantified across the three years. This work demonstrates that NPS are used across different continents and countries with the use of some more evident in particular regions. For example, mitragynine has highest mass loads in sites in the United States, while eutylone and 3-methylmethcathinone increased considerably in New Zealand and in several European countries, respectively. Moreover, 2F-deschloroketamine, an analogue of ketamine, has emerged more recently and could be quantified in several sites, including one in China, where it is considered as one of the drugs of most concern. Finally, some NPS were detected in specific regions during the initial sampling campaigns and spread to additional sites by the third campaign. Hence, wastewater surveillance can provide an insight into temporal and spatial trends of NPS use.

Abstract Background A zirconium-based metal-organic framework (Zr-MOF), named MOF-808, was synthesized and fully characterized by solvo-thermal method and functionalized by isonicotinic acid and employed as an efficient adsorbent for selective extraction and preconcentration of uranyl ions from water and waste water samples in a batch solid phase extraction. Results Parameters affecting extraction such as volume and pH of the sample solution, the amount of sorbent, type and volume of eluting solvent, and adsorption and desorption times were investigated and optimized. Under the optimized conditions, high extraction efficiency was observed with a limit of detection of 0.9 µg L− 1 for uranyl ions and relative standard deviations were found to be better than 2.1% in the range of 0.07–1000 µg L− 1. Conclusions These results indicated that the above procedure is fast, inexpensive, effective, reliable, applicable and organic solvent-free and showed the highly performance and stability of the Zr-MOF in SPE based analytical techniques.

Background: The genomes of SARS-CoV-2 are classified into variants, some of which are monitored as variants of concern (e.g. the Delta variant B.1.617.2 or Omicron variant B.1.1.529). Proportions of these variants circulating in a human population are typically estimated by large-scale sequencing of individual patient samples. Sequencing a mixture of SARS-CoV-2 RNA molecules from wastewater provides a cost-effective alternative, but requires methods for estimating variant proportions in a mixed sample. Results: We propose a new method based on a probabilistic model of sequencing reads, capturing sequence diversity present within individual variants, as well as sequencing errors. The algorithm is implemented in an open source Python program called VirPool. We evaluate the accuracy of VirPool on several simulated and real sequencing data sets from both Illumina and nanopore sequencing platforms, including wastewater samples from Austria and France monitoring the onset of the Alpha variant. Conclusions: VirPool is a versatile tool for wastewater and other mixed-sample analysis that can handle both short- and long-read sequencing data. Our approach does not require pre-selection of characteristic mutations for variant profiles, it is able to use the entire length of reads instead of just the most informative positions, and can also capture haplotype dependencies within a single read. [ABSTRACT FROM AUTHOR]

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Sustainability in the textile industry is a challenge with an imminent need to be tackled. One approach can be focused on replacing fossil-based dyes with renewable and less polluting alternatives. In this sense, this study focuses on validating the suitability of an innovative natural-based blue dye, phycocyanin, sourced from Spirulina platensis microalgae. The laboratory-based experimental approach envisages the exhaustion dyeing of pre-mordanted cotton and bleached wool with phycocyanin-rich extract, representing the sustainable blue dye. The color characterization of naturally blue-dyed fabrics was performed via CIE Lab coordinates, depth of color by color stregth valures (K/S), values of dye exhaustion, and colorfastness to laundering and light. The results indicate suitable dyeability with the natural blue dye, with process improvements a possibility. The main environmental character of this process was analyzed from the dyeing effluent characterization perspective. Measurements of chemical oxygen demand, biochemical oxygen demand, and metal content were performed on effluents resulting from dyeing processes with variable parameters, to analyze the influence of mordant use, process temperature, time, and pH. Findings indicate that the application of optimum dyeing process conditions results in the lowest oxygen demand values, suitable for further wastewater reuse, according to international industrial effluent limitations. The biological fungi wastewater treatment resulted in the reduction of biochemical oxygen demand and chemical oxygen demand values by around 80%, comparable with the industrial process, validating the sustainable character of using algae-based phycocyanin in the bath exhaustion dyeing process. [ABSTRACT FROM AUTHOR]

New psychoactive substances (NPS) are of public health concern due to their sporadic proliferation and the dearth of information on toxicity when consumed. In addition to seized data from forensic and toxicology reporting, wastewater analysis serves as a complimentary tool for NPS surveillance. A method to detect 71 NPS by simple filtration followed by liquid-chromatography tandem mass spectrometry was developed to detect multiclass NPS consisting of arylcyclohexylamines, designer benzodiazepines, synthetic cannabinoids, synthetic opioids, phenethylamines, synthetic cathinones, tryptamines, and indole alkaloids. In this work, the influential factors for electrospray ionisation were identified and optimised using the fractional factorial design and face-centred central composite design, respectively. The filtration loss during sample clean-up was assessed for all compounds. The final method was validated and applied to wastewater collected from a music festival held in Queensland in 2022. The validated method had linearity between 0.5 ng L−1 and 5000 ng L−1, the limit of quantification (LOQ) ranges from 0.6 ng L−1 to 70 ng L−1, precision within ±20 %, accuracy ranges from 70 % to 120 %, and matrix effect ranges from soft (0 %–20 %) to medium (20 %–50 %) for the majority of the compounds. NPS detected in the festival were 2-fluorodeschloroketamine, 7-hydroxymitragynine, mitragynine, N,N -dimethylpentylone, pentylone, phenibut, and O- desmethyltramadol. Systematic electrospray ionisation optimisation using the design of experiment for a large method is practical and provides in-depth chemical information on studied compounds. The optimised method demonstrated the applicability of analysing samples collected from a festival in this work. [Display omitted] • A high throughput method was developed for 71 new psychoactive substances. • Important variables for optimisation were temperature, ion source gas, and ion source voltage. • Seven compounds were detected in samples collected from a festival. [ABSTRACT FROM AUTHOR]

• Structured chromatograms improve reliability of compound identification. • Improved mass spectral quality in pulsed elution-LC × LC-HRMS. • Better understanding retention in the pulsed elution-LC × LC. • Improved pulse shape control and accuracy at low pulse volumes. • Flexible method development in pulsed elution-LC × LC. Due to the decoupling of the first (1D) and second (2D) dimension in pulsed elution-LC × LC (PE-LC × LC), method development is more flexible and straightforward compared to fast comprehensive LC × LC where the dependencies of key parameters between the two dimensions limits its flexibility. In this study we present a method for pulse generation, which is based on a switching valve alternating between one pump that delivers the gradient and a second pump that delivers low eluotrophic strength for the pause state. Consequently, the dwell volume of the system was circumvented and 7.5, and 3.75 times shorter pulse widths could be generated at flow rates of 0.2, and 0.4 mL/min with satisfactory accuracies between programmed and observed mobile phase composition (relative deviation of 6.0 %). We investigated how key parameters including pulse width and step height, 2D gradient time and flow rate affected the peak capacity in PE-LC × LC. The conditions yielding the highest peak capacity for the PE-LC × LC- high-resolution mass spectrometry (HRMS) system were applied to a wastewater effluent sample. The results were compared to a one dimensional (1D)-LC-HRMS chromatogram. The peak capacity increased with a factor 34 from 112 for the 1D-LC run to 3770 for PE-LC × LC-HRMS after correction for undersampling. The analysis time for PE-LC × LC-HRMS was 12.1 h compared to 67.5 min for the 1D-LC-HRMS run. The purity of the mass spectra improved for PE-LC × LC-HRMS by a factor 2.6 (p-value 3.3 × 10−6) and 2.0 (p-value 2.5 × 10−3) for the low and high collision energy trace compared to the 1D-LC-HRMS analysis. Furthermore, the signal-to-noise ratio (S/N) was 4.2 times higher (range: 0.06–56.7, p-value 3.8 × 10−2) compared to the 1D-LC-HRMS separation based on 42 identified compounds. The improvements in S/N were explained by the lower peak volume obtained in the PE-LC × LC-HRMS. [ABSTRACT FROM AUTHOR]

In this study, we developed a novel on-line solid phase extraction (SPE)-ultra-high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS)-based analytical method for simultaneously quantifying 12 illicit drugs and metabolites (methamphetamine, amphetamine, morphine, codeine, 6-monoacetylmorphine, benzoylecgonine, 3,4-methylenedioxymethamphetamine, 3,4-methylenedioxyamphetamine, cocaine, ketamine, norketamine, and methcathinone) and cotinine (COT) in wastewater samples. The analysis was performed by loading 2 mL of the sample onto an Oasis hydrophilic-lipophilic balance cartridge and using a cleanup step (5% methanol) to eliminate interference with a total run time of 13 min. The isotope-labeled internal standard method was used to quantify the target substances and correct for unavoidable losses and matrix effects during the on-line SPE process. Typical analytical characteristics used for method validation were sensitivity, linearity, precision, repeatability, recovery, and matrix effects. The limit of detection (LOD) and limit of quantification (LOQ) of each target were set at 0.20 ng/L and 0.50 ng/L, respectively. The linearity was between 0.5 ng/L and 250 ng/L, except for that of COT. The intra- and inter-day precisions were

This study aims to optimize a single preparation methodology based on solid-phase extraction (SPE) that could fit both target and non-target screening of organic biomarkers in raw wastewater, allowing the cross-comparison of results obtained from a same dataset. The efficiency of SPE sorbents used alone (HLB) or in combination in a multilayer cartridge was evaluated based on (i) the extraction recovery and matrix effect in environmental samples (surface water and wastewater) for a list of biomarkers (pharmaceuticals, licit and illicit drugs, artificial sweeteners, isoprostanes, polyphenols) and (ii) a number of detected features and their intensity in HRMS. The selected method uses a combination of three SPE sorbents mixed together (HLB, X-AW and X-CW) and seems to take full advantage of each, providing satisfactory validation parameters (recovery, instrumental limit of detection, linearity range and limit of quantification) over a large range of physico-chemical properties while ensuring promising results for non-target screening applications. Of the 65 targeted compounds, nearly all of them (47) were detected in wastewater influent samples with concentration above the limit of quantification, while at the same time over 10 000 features were recorded according to the high resolution mass spectrometry (HRMS) fingerprint, holding out the promise that a common protocol for these two analyses, with their very contrasting constraints and objectives, is possible.

Wastewater treatment plants (WWTPs) can benefit from utilizing digital technologies to reduce greenhouse gas (GHG) emissions and to comply with effluent quality standards. In this study, the GHG emissions and electricity consumption of a WWTP were evaluated via computer simulation by varying the dissolved oxygen (DO), mixed liquor recirculation (MLR), and return activated sludge (RAS) parameters. Three different measures, namely, effluent water quality, GHG emissions, and energy consumption, were combined as water-energy-carbon coupling index (WECCI) to compare the effects of the parameters on WWTPs, and the optimal operating condition was determined. The initial conditions of the A2O process were set to 4.0 mg/L of DO, 100 % MLR, and 90.7 % RAS. Eighty scenarios with various DO, MLR, and RAS were simulated under steady-state condition to optimize the biological treatment process. The optimal operating conditions were found to be 1.5 mg/L of DO, 190 % MLR, and 90.9 % RAS, which had the highest WECCI of 2.40 when compared to the WECCI of the initial condition (1.07). This optimal condition simultaneously reduced GHG emissions by 1348 kg CO 2 -eq/d and energy consumption by 11.64 MWh/d. This implies that controlling DO, MLR, and RAS through sensors, valves, and pumps offers a promising approach to operating WWTPs with reduced electricity consumption and GHG emissions while attaining effluent quality standards. Additionally, the nitrous oxide stripping rate exhibited linear relationships with the effluent total ammonia and nitrite concentrations in the aerobic reactor, suggesting that monitoring dissolved nitrogen compounds in the effluent and reactor could be a viable strategy to control MLR and DO in the biological reactor. The digital-based assessment and optimization tools developed in this study are expected to hold promise for application in broader environmental management efforts., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 The Authors. Published by Elsevier Inc. All rights reserved.)

In an attempt to discover and characterize the plethora of xenobiotic substances, this study investigates chemical compounds released into the environment with wastewater effluents. A novel non-targeted screening methodology based on ultra-high resolution Orbitrap mass spectrometry and nanoflow ultra-high performance liquid chromatography together with a newly optimized data-processing pipeline were applied to effluent samples from two state-of-the-art and one small wastewater treatment facility. In total, 785 molecular structures were obtained, of which 38 were identified as single compounds, while 480 structures were identified at a putative level. Most of these substances were therapeutics and drugs, present as parent compounds and metabolites. Using R packages Phyloseq and MetacodeR, originally developed for bioinformatics, significant differences in xenobiotic presence in the wastewater effluents between the three sites were demonstrated., Competing Interests: Declaration of competing interest The authors declare no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 The Authors. Published by Elsevier Inc. All rights reserved.)

The extensive use of insecticides, such as pyrethroids, and pharmaceutical drugs, such as doxorubicin (DOX) has significantly increased to meet the growing demand for food production and disease treatment. Among them, 3-phenoxybenzoic acid (3-PBA), a metabolite of pyrethroid insecticides, poses various health and environmental risks. Similarly, DOX is a well-known anticancer drug and has been continuously used for many years. The high demand and unregulated disposal of these substances raise concerns for both humans and the environment. To address this issue, there is a pressing need to monitor the presence of these analytes in wastewater to protect our ecosystems. This challenge has inspired us to develop an MOF-based fluorometric dual sensor capable of rapid and selective detection of these analytes in aqueous solutions. This work represents the first MOF-based dual probe for detecting these targeted analytes. There was a 98% fluorescence quenching upon the introduction of DOX whereas about a 11-fold increment of the probe's fluorescence intensity took place in the presence of 3-PBA. The sensitivity of the probe is notably high as limits of detection (LOD) are 8.7 nM for DOX and 1.2 nM for 3-PBA. Our designed probe has the highest K SV value for DOX which is 3.37 × 10 6 M -1 . The MOF demonstrated remarkable rapid response time of just 5 and 10 s for DOX and 3-PBA, respectively. The MOF exhibited outstanding selectivity in detecting DOX and 3-PBA, even when other interfering substances were present. We tested the probe's sensing abilities in various environments, such as serum, urine, wastewater, and different pH levels. These findings underscore the sensor's practicality and usefulness in real-world applications. The underlying mechanisms driving the sensing processes were thoroughly investigated by using various modern analytical methods.

Knowledge of the number of people present in a catchment is fundamental for the assessment of spatio-temporal trends in wastewater-based epidemiology (WBE). Accurately estimating the number of people connected to wastewater catchments is challenging however, because populations are dynamic. Methods used to estimate population size can significantly influence the calculation and interpretation of population-normalised wastewater data (PNWD). This paper systematically reviews the reporting of population data in 339 WBE studies. Studies were evaluated based on their reporting of population size, the source of population data, the population calculation methods, and the uncertainties in population estimates. Most papers reported population size (96 %) and the source of population data (60 %). Fewer studies reported the uncertainties in their population data (50 %) and the methods used to calculate these estimates (28 %). This is relevant because different methods have unique strengths and limitations which can affect the accuracy of PNWD. Only 64 studies (19 %) reported all four components of population data. The reporting of population data has remained consistent in the past decade. Based on the findings, we recommend generalised reporting criteria for population data in WBE. As WBE is further mainstreamed and applied, the clear and comprehensive reporting of population data will only become increasingly important., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 The Authors. Published by Elsevier B.V. All rights reserved.)

Emerging contaminants pose a potential risk to aquatic ecosystems in the Pearl River Basin, China, owing to the high population density and active industry. This study investigated samples from eight sewage treatment plants, and five surface water bodies of related watersheds. To screen the risk of emerging contaminants (ECs), and clarify their sources, this study calculated the risk quotient of detected chemical and performed source identification/apportionment using the positive matrix factorization method. In total, 149 organic pollutants were identified. Pharmaceuticals showed significant concentrations in sewage treatment plant samples (120.87 ng/L), compared with surface water samples (1.13 ng/L). The ecological risk assessment identified three chemicals with a heightened risk to aquatic organisms: fipronil sulfide, caffeine, and roxithromycin. Four principal sources of contaminants were identified: pharmaceutical wastewater, domestic sewage, medical effluent, and agricultural runoff. Pharmaceutical wastewater was the primary contributor (60.4 %), to the cumulative EC concentration and to ECs in sewage treatment plant effluent. Agricultural drainage was the main source of ECs in surface water. This study provides a strategy to obtain comprehensive information on the aquatic risks and potential sources of EC species in areas affected by artificial activities, which is of substantial importance to pollutant management and control., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)

Currently, there is uncertainty about emissions of pharmaceuticals into larger closed ecosystems that are at risk such as the Baltic Sea. There is an increasing need for selecting the right strategies on advanced wastewater treatment. This study analysed 35 pharmaceuticals and iodinated X-ray contrast media in effluents from 82 Wastewater Treatment Plants (WWTPs) across Denmark, Estonia, Finland, Germany, Latvia, Lithuania, Poland and Sweden. Measured concentrations from Finland and Denmark were compared to predicted effluent concentrations using different levels of refinement. The concentrations predicted by the Total Residue Approach, as proposed by the European Medicines Agency, correlated with R 2 of 0.18 and 0.031 to measured ones for Denmark and Finland, respectively and the predicted data were significantly higher than the measured ones. These correlations improved substantially to R 2 of 0.72 and 0.74 after adjusting for estimated human excretion rates and further to R 2 = 0.91 and 0.78 with the inclusion of removal rates in WWTPs. Temporal analysis of compound variations in a closely monitored WWTP showed minimal fluctuation over days and weeks for most compounds but revealed weekly shifts in iodinated X-ray contrast media due to emergency-only operations at X-ray clinics during weekends and an abrupt seasonal change for gabapentin. The findings underscore the limitations of current predictive models and findings (...) demonstrate how these methodologies can be refined by incorporating human pharmaceutical excretion/metabolization as well as removal in wastewater treatment plants to more accurately forecast pharmaceutical levels in aquatic environments., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 The Authors. Published by Elsevier B.V. All rights reserved.)

Neonicotinoid pesticides are a relatively new class of pesticides that have garnered significant attention owing to their potential ecological risks to nontarget organisms. A method combining solid phase extraction with liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) was developed for the rapid and accurate detection of eight neonicotinoid pesticides (dinotefuran, E -nitenpyram, thiamethoxam, clothianidin, imidacloprid, imidaclothiz, acetamiprid, and thiacloprid) in wastewater. The chromatographic mobile phase and MS parameters were selected, and a single-factor method was used to determine the optimal column type, extraction volume, sample loading speed, and pH for SPE. The optimal parameters were as follows: column type, HLB column (500 mg/6 mL); sample extraction volume, 500 mL; sample loading speed, 10 mL/min; and sample pH, 6-8. The matrix effects of the wastewater samples were reduced by optimizing the chromatographic gradient-elution program, examining the dilution factor of the samples, and using the isotope internal standard calibration method. Prior to analysis, the wastewater samples were diluted 5-fold with ultrapure water for pretreatment. Subsequently, 2 mmol/L ammonium acetate aqueous solution containing 0.1% (v/v) formic acid and methanol was used as mobile phases for gradient elution on a ZORBAX Eclipse Plus C18 column (100 mm×2.1 mm, 1.8 μm). The samples were quantified using positive-ion multiple reaction monitoring (MRM) mode for 10 min. Imidacloprid-d4 was used as the isotope internal standard. The SPE process was further optimized by applying response surface methodology to select the type and mass of rinsing and elution solvents. The optimal pretreatment of the SPE column included rinsing with 10% methanol aqueous solution and elution with methanol-acetonitrile (1∶1, v/v) mixture (7 mL). The eight neonicotinoid pesticides showed satisfactory linearity within the relevant range, with linear correlation coefficients ( r ) all greater than 0.9990. The method detection limits (MDLs) ranged from 0.2 to 1.2 ng/L, and the method quantification limits (MQLs) ranged from 0.8 to 4.8 ng/L. The average recoveries of the eight neonicotinoid pesticides were in the range of 82.6%-94.2% at three spiked levels, with relative standard deviations (RSDs) ranging from 3.9% to 9.4%. Finally, the optimized method was successfully applied to analyze wastewater samples collected from four sewage treatment plants. The results indicated that the eight neonicotinoid pesticides could be generally detected at concentrations ranging from not detected (ND) to 256 ng/L. The developed method has a low MDL and high accuracy, rendering it a suitable choice for the trace detection of the eight neonicotinoid pesticides in wastewater when compared with other similar methods. The proposed method can be utilized to monitor the environmental impact and assess the potential risks of neonicotinoid pesticides in wastewater, thus promoting the protection of nontarget organisms and the sustainable use of these pesticides in agriculture.

Background: An increasing number of β 2 -adrenergic agonists are illicitly used for growth promoting and lean meat increasing in animal husbandry in recent years, but the development of analytical methods has lagged behind these emerging drugs., Results: Here, we designed and developed an ultrasound probe enhanced enzymatic hydrolysis reactor for quick separation and simultaneously quantification of 22 β 2 -adrenergic agonists in animal urine and livestock wastewater. Owing to the enhancement of the conventional enzymatic digestion through the ultrasound acoustic probe power, only 2 min was required for the comprehensively separation of β 2 -adrenergic agonists from the sample matrices, making it a much more desirable alternative tool for high-throughput investigation. The swine, bovine and sheep urines (n = 287), and livestock wastewater (n = 15) samples, collected from both the north and south China, were examined to demonstrate the feasibility and capability of the proposed approach. Six kinds of β 2 -adrenergic agonists (clenbuterol, salbutamol, ractopamine, terbutaline, clorprenaline and cimaterol) were found in animal urines, with concentrations ranged between 0.056 μg/L (terbutaline) and 5.79 μg/L (clenbuterol). Up to nine β 2 -adrenergic agonists were detected in wastewater samples, of which four were found in swine farms and nine in cattle/sheep farms, with concentration levels from 0.069 μg/L (tulobuterol) to 2470 μg/L (clenbuterol)., Significance: Interestingly, since β 2 -adrenergic agonists are usually considered to be abused mainly in the pig farms, our data indicate that both the detection frequencies and concentrations of these agonists in the ruminant farms were higher than the pig farms. Furthermore, the findings of this work indicated that there is a widespread occurrence of β 2 -adrenergic agonists in livestock farms, especially for clenbuterol and salbutamol, which may pose both food safety and potential ecological risks. We recommend that stricter controls should be adopted to prevent the illegally usage of these β 2 -adrenergic agonists in agricultural animals, especially ruminants, and they should also be removed before discharging to the environment., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)

Microalgae are a promising bio-fertilizer that can be cultivated in municipal wastewater, where the organisms perform water purification by incorporation of nutrients and contaminants. Before bio-fertilization with wastewater-grown microalgae can be put into practice, its impact on the leaching of macronutrients and trace elements needs to be evaluated. Here, we studied the leaching behavior of a microalgae-fertilized soil against a control in column percolation setup. Microalgae were grown in real municipal wastewater supplemented with bromide for the analysis of within-cell Br - accumulation by time-of-flight secondary ion mass spectrometry. Dry biomass (45.0 g N kg -1 and 28.9 g P kg -1 ) was added to the topmost layer of the fertilized column at a level of 3 g biomass kg -1 on a whole soil basis. Column irrigation was equivalent to 3 years of precipitation in central Germany. The leaching of macronutrients and trace elements from the fertilized and control columns was largely identical. Except for P, depth profiles confirmed very low vertical translocation within the soil. This is held for total element contents as well as for operationally defined pools, suggesting that microalgae cultivated in municipal wastewater provide a slow-release fertilizer largely resistant to leaching. Mass spectrometric imaging gave clear evidence for bromide uptake by the microalgae, and pure cultures of the genus Scenedesmus showed that it was preferentially located in the cell membrane. Therefore, bromide could potentially be employed as a mineralization tracer in future studies on the use of microalgae as a bio-fertilizer., (© 2024 The Author(s). Journal of Environmental Quality published by Wiley Periodicals LLC on behalf of American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America.)

Antibiotics are widely used as fungicides because of their antibacterial and bactericidal effects. However, it is necessary to control their dosage. If the amount of antbiotics is too much, it cannot be completely metabolized and absorbed, will pollute the environment, and have a great impact on human health. Many antibiotics usually left in factory or aquaculture wastewater pollute the environment, so it is vital to detect the content of antibiotics in wastewater. This article summarizes several common methods of antibiotic detection and pretreatment steps. The detection methods of antibiotics in wastewater mainly include immunoassay, instrumental analysis method, and sensor. Studies have shown that immunoassay can detect deficient concentrations of antibiotics, but it is affected by external factors leading to errors. The detection speed of the instrumental analysis method is fast, but the repeatability is poor, the price is high, and the operation is complicated. The sensor is a method that is currently increasingly studied, including electrochemical sensors, optical sensors, biosensors, photoelectrochemical sensors, and surface plasmon resonance sensors. It has the advantages of fast detection speed, high accuracy, and strong sensitivity. However, the reproducibility and stability of the sensor are poor. At present, there is no method that can comprehensively integrate the advantages. This paper aims to review the enrichment and detection methods of antibiotics in wastewater from 2020 to the present. It also aims to provide some ideas for future research directions in this field., (© 2024. The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature.)

Pesticides pose a significant threat to aquatic ecosystems due to their persistent nature and adverse effects on biota. The increased detection of pesticides in various water bodies has prompted research into their toxicological impacts and potential remediation strategies. However, addressing this issue requires the establishment of robust regulatory frameworks to determine safe thresholds for pesticide concentrations in water and the development of effective treatment methods. This assessment underscores the complex ecological risks associated with organophosphate pesticides (OPPs) and emphasizes the urgent need for strategic management and regulatory measures. This study presents a detailed examination of the global prevalence of OPPs and their potential adverse effects on aquatic and human life. A comprehensive risk assessment identifies azinphos-methyl, chlorpyrifos, and profenfos as posing considerable ecological hazard to fathead minnow, daphnia magna, and T. pyriformis. Additionally, this review explores the potential efficacy of constructed wetlands (CWs) as a sustainable approach for mitigating wastewater contamination by diverse pesticide compounds. Furthermore, the review assess the effectiveness of CWs for treating wastewater contaminated with pesticides by critically analyzing the removal mechanism and key factors. The study suggests that the optimal pH range for CWs is 6-8, with higher temperatures promoting microbial breakdown and lower temperatures enhancing pollutant removal through adsorption and sedimentation. The importance of wetland vegetation in promoting sorption, absorption, and degradation processes is emphasized. The study emphasizes the importance of hydraulic retention time (HRT) in designing, operating, and maintaining CWs for pesticide-contaminated water treatment. The removal efficiency of CWs ranges from 38% to 100%, depending on factors like pesticide type, substrate materials, reactor setup, and operating conditions., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

Sustainability and life-cycle concerns about the conventional activated sludge (CAS) process for wastewater treatment have been driving the development of energy-efficient, greener alternatives. Feasibility of an algal-based wastewater treatment (A-WWT) system has been demonstrated recently as a possible alternative, capable of simultaneous nutrient and energy recovery. This study compared capabilities of the A-WWT and CAS systems in removing organic micropollutants (OMP). Initial assessments based on surrogate organic measures and fluorescence excitation-emission matrix (FEEM) scans revealed that the A-WWT system achieved higher removals of organics than the CAS system. However, effluents of both systems contained residual organic matter, necessitating further OMP assessment for a rigorous comparison. A novel ultrahigh-performance liquid chromatography- Fourier transform mass spectrometry (UPLC-FTMS)-based non-targeted screening approach was adopted here for residual OMP analysis. This approach confirmed that the A-WWT system resulted in better OMP removal, eliminating 329 compounds and partially reducing 472 compounds, compared to 206 eliminations and 410 partial reductions by the CAS system. Mass spectra signal corresponding to some OMPs increased with treatment while some transformation products were observed following treatment. Higher OMP reduction in the A-WWT system with concurrent reductions of biodegradable carbon, nutrients, and pathogens in a single-step while producing energy and nutrient rich algal biomass underscore its potential as a greener alternative for wastewater treatment., Competing Interests: Declaration of competing interest The authors declare no competing financial interest., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

Tobacco-specific alkaloids and nitrosamines are important biomarkers for the estimation of tobacco use and human exposure to tobacco-specific nitrosamines that can be monitored by wastewater analysis. Thus far their analysis has used solid phase extraction, which is costly and time-consuming. In this study, we developed a direct injection liquid chromatography-tandem mass spectrometry method for the quantification of two tobacco-specific alkaloids and five nitrosamines in wastewater. The method achieved excellent linearity (R 2  > 0.99) for all analytes, with calibration ranging from 0.10 to 800 ng/L. Method limits of detection and quantification were 0.17 ng/L (N-nitrosonornicotine, NNN) and 1.0 ng/L (N-nitrosoanatabine (NAT) and NNN), with acceptable accuracy (100 % ± 20 %) and precision (± 15 %). Analyte loss during filtration was < 15 %, and the relative matrix effect was < 10 %. The method was applied to 43 pooled wastewater samples collected from three wastewater treatment plants in Australia between 2017 and 2021. Anabasine and anatabine were detected in all samples at concentrations of 5.0 - 33 ng/L and 12 - 41 ng/L, respectively. Three of the five tobacco-specific nitrosamines (NAT, NNN, and (4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol) (NNAL)) were detected, in < 50 % of the wastewater samples, with concentrations nearly ten times lower than the tobacco alkaloids (< 1.0 - 6.2 ng/L). In-sewer stability of the nitrosamines was also assessed in this study, with four (NAT, NNAL, NNN, and N-nitrosoanabasine (NAB)) being stable (i.e. < 20 % transformation over 12 h in both control reactor (CR) and rising main reactor (RM) and 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone (NNK) being moderately stable (< 40 % loss over 12 h in RM). This direct injection method provides a high-throughput approach in simultaneous investigation of tobacco use and assessment of public exposure to tobacco-specific nitrosamines., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024. Published by Elsevier B.V.)

An electrochemical aptasensor was developed by utilizing a DNA walker driven by catalytic hairpin assembly (CHA) with kanamycin as the model analyte. Kanamycin bound to the aptamer, causes the release of DNA walker, triggers the CHA reaction, leads to the cyclic movement of the walker's long arm, and results in cascade amplification of the signal. The guanine-rich sequences of the double-stranded products produced by CHA were folded to form G-quadruplex structures, with electrochemical active molecules Hemin embedded, forms G-quadruplex/Hemin complexes in situ on the electrode surface, thereby achieving sensitive, efficient, and label-free detection of kanamycin with a limit of detection (LOD) of 0.27 pM (S/N = 3). Meaningfully, the aptasensor demonstrated high sensitivity and reliability in the detection of kanamycin in milk and livestock wastewater samples, suggesting that it has great potential for application in detecting antibiotics in food products and water samples from the environment., (© 2024. The Author(s), under exclusive licence to Springer-Verlag GmbH Austria, part of Springer Nature.)

Aromatic amines (AAs) are human-made compounds known for their mutagenic properties, entering surface waters from various sources, often originating as transformation products of dyes or pesticides. Despite their low concentrations in surface waters, AAs can exhibit mutagenicity. Our study focused on evaluating three passive samplers (PSs) for enriching these compounds from influent and effluent of a wastewater treatment plant (WWTP) in Brno, Czech Republic. The PSs tested included variants containing AttractSPE™ SDB-RPS sorbent disk, one with and one without a diffusive agarose hydrogel layer, and a modified Speedisk (Bakerbond Speedisk® H 2 O-Philic). PSs were deployed in wastewater (WW) for one to four weeks in various overlapping combinations, and the uptake of AAs to PSs was compared to their concentrations in 24-hour composite water samples. A targeted LC/MS analysis covered 42 amines, detecting 11 and 13 AAs in daily composite influent and effluent samples, respectively. In the influent, AAs ranged from 1.5 ng L -1 for 1-anilinonaphthalene to 1.0 μg L -1 for aniline, and the highest concentration among all measured amines was observed for cyclohexylamine at 2.9 μg L -1 . In the effluent, concentrations ranged from 0.5 ng L -1 for 1-anilinonaphthalene to 88 ng L -1 for o-anisidine. PSs demonstrated comparable accumulation of amines, with integrative uptake up to 28 days in both influent and effluent and detection of up to 23 and 27 amines in influent and effluent, respectively; altogether 34 compounds were detected in the study. Sampling rates (R s ) were estimated for compounds present in at least 50 % of the samples and showing <40 % aqueous concentration variability, with robustness evaluated by comparing values for compounds in WWTP influent and effluent. Although all devices performed similarly, hydrogel-based PS exhibited superior performance in several criteria, including time integration and robustness of sampling rates, making it a suitable monitoring tool for AAs in WW., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)

Background: Many countries have applied the wastewater surveillance of the COVID-19 pandemic to their national public health monitoring measures. The most used methods for detecting SARS-CoV-2 in wastewater are quantitative reverse transcriptase-polymerase chain reaction (RT-qPCR) and reverse transcriptase-droplet digital polymerase chain reaction (RT-ddPCR). Previous comparison studies have produced conflicting results, thus more research on the subject is required., Objective: This study aims to compare RT-qPCR and RT-ddPCR for detecting SARS-CoV-2 in wastewater. It also aimed to investigate the effect of changes in the analytical pipeline, including the RNA extraction kit, RT-PCR kit, and target gene assay, on the results. Another aim was to find a detection method for low-resource settings., Methods: We compared 2 RT-qPCR kits, TaqMan RT-qPCR and QuantiTect RT-qPCR, and RT-ddPCR based on sensitivity, positivity rates, variability, and correlation of SARS-CoV-2 gene copy numbers in wastewater to the incidence of COVID-19. Furthermore, we compared 2 RNA extraction methods, column- and magnetic-bead-based. In addition, we assessed 2 target gene assays for RT-qPCR, N1 and N2, and 2 target gene assays for ddPCR N1 and E. Reverse transcription strand invasion-based amplification (RT-SIBA) was used to detect SARS-CoV-2 from wastewater qualitatively., Results: Our results indicated that the most sensitive method to detect SARS-CoV-2 in wastewater was RT-ddPCR. It had the highest positivity rate (26/30), and its limit of detection was the lowest (0.06 gene copies/µL). However, we obtained the best correlation between COVID-19 incidence and SARS-CoV-2 gene copy number in wastewater using TaqMan RT-qPCR (correlation coefficient [CC]=0.697, P<.001). We found a significant difference in sensitivity between the TaqMan RT-qPCR kit and the QuantiTect RT-qPCR kit, the first having a significantly lower limit of detection and a higher positivity rate than the latter. Furthermore, the N1 target gene assay was the most sensitive for both RT-qPCR kits, while no significant difference was found between the gene targets using RT-ddPCR. In addition, the use of different RNA extraction kits affected the result when the TaqMan RT-qPCR kit was used. RT-SIBA was able to detect SARS-CoV-2 RNA in wastewater., Conclusions: As our study, as well as most of the previous studies, has shown RT-ddPCR to be more sensitive than RT-qPCR, its use in the wastewater surveillance of SARS-CoV-2 should be considered, especially if the amount of SARS-CoV-2 circulating in the population was low. All the analysis steps must be optimized for wastewater surveillance as our study showed that all the analysis steps including the compatibility of the RNA extraction, the RT-PCR kit, and the target gene assay influence the results. In addition, our study showed that RT-SIBA could be used to detect SARS-CoV-2 in wastewater if a qualitative result is sufficient., (©Annika Länsivaara, Kirsi-Maarit Lehto, Rafiqul Hyder, Erja Sinikka Janhonen, Anssi Lipponen, Annamari Heikinheimo, Tarja Pitkänen, Sami Oikarinen, WastPan Study Group. Originally published in JMIR Public Health and Surveillance (https://publichealth.jmir.org), 19.08.2024.)

Wastewater (WW)-based epidemiology is an approach for the objective surveillance of the consumption of (illicit) drugs in populations. The aims of this study were to monitor drugs of abuse, cognitive enhancers, and their metabolites as biomarkers in influent WW. Data obtained from different sampling points and mean daily loads were compared with previously published data. The prevalence of analytes was monitored in WW grab samples collected monthly over 22 months at two sampling points and 24 h composite WW samples collected over 2 weeks at a WW treatment plant in the same city. Quantification was performed using a previously validated and published method based on solid-phase extraction followed by liquid chromatography coupled with high-resolution tandem mass spectrometry. Grab samples allowed for frequent detection of ritalinic acid and sporadic detection of drugs of abuse. The daily mean loads calculated for 24 h WW composite samples were in accordance with data published in an international study. Furthermore, loads of amphetamine and methamphetamine increased compared with those observed in a previously published study from 2014. This study showed frequent quantification of ritalinic acid in the grab samples, while drugs of abuse were commonly quantified in the composite WW samples. Daily mean loads were in accordance with trends reported for Germany.

This study evaluates the effectiveness of self-assessed exposure (SAE) data collection for characterization of hydrogen sulfide (H2S) risks in water and wastewater management, challenging the adequacy of traditional random or campaign sampling strategies. We compared 3 datasets derived from distinct strategies: expert data with activity metadata (A), SAE without metadata (B), and SAE with logbook metadata (C). The findings reveal that standard practices of random sampling (dataset A) fail to capture the sporadic nature of H2S exposure. Instead, SAE methods enhanced by logbook metadata and supported by reliable detection and calibration infrastructure (datasets B and C) are more effective. When assessing risk, particularly peak exposure risks, it is crucial to adopt measures that capture exposure variability, such as the range and standard deviations. This finer assessment is vital where high H2S peaks occur in confined spaces. Risk assessment should incorporate indices that account for peak exposure, utilizing variability measures like range and standard or geometric standard deviation to reflect the actual risk more accurately. For large datasets, a histogram is just as useful as statistical measures. This approach has revealed that not only wastewater workers but also water distribution network workers, can face unexpectedly high H2S levels when accessing confined underground spaces. Our research underscores the need for continuous monitoring with personal electrochemical gas detector alarm systems, particularly in environments with variable and potentially hazardous exposure levels., (© The Author(s) 2024. Published by Oxford University Press on behalf of the British Occupational Hygiene Society.)

Municipal wastewater treatment plants are required to monitor persistent organic pollutants (POPs) in their wastewater treatment related discharges and to assess the impact of the discharges on the environment and public health. One tool for monitoring chlorinated organic pollutants particularly is a gas chromatographic (GC) system coupled to a pair of halogen-specific electron capture detectors (ECDs) with helium (He) as the mobile phase. He supplies, however, has become inconsistent and unreliable lately. In its place, N 2 gas is evaluated in this study as a potential substitute for He in quantifying organochlorine pesticides, polychlorinated biphenyls, chlordane congeners and toxaphene in wastewater treatment related matrices (influent, effluent, benthic sediment, mussel tissue, and biosolids/sludge). N 2 is inert, inexpensive and requires no additional hardware to incorporate into the basic functions of a GC-ECD. Our results show that, with the usual data quality controls (blank, laboratory control, matrix spike/duplicate and proficiency testing samples, and the fact that certified reference materials data met requirements), N 2 can replace He for regulatory purposes. And when necessary, the N 2 -based retention times (t N ) can be predicted reliably from He-based retention times (t He ), irrespective of column chemistry or POPs (here: t N = 1.90t He + 0.04, R 2 = 0.996)., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper, (Copyright © 2024 Elsevier B.V. All rights reserved.)

National opinions on a wide variety of public health topics can change over time and have highly contextual nuances. This study is a follow-up to prior inquiries into the knowledge of wastewater-based epidemiology, privacy concerns surrounding sample collection, and the use of data acquired, along with privacy awareness from an online survey conducted in the metropolitan United States during the winter of 2023. Mentions of wastewater-surveillance-related terms in the media remained common. Towards the outbreak tail in 2023, public support for surveillance of toxins (91%), diseases (91%), terrorist threats (87%), illicit drugs (70%), prescription medications (69%), and gun residue (60%) remained high. There was less support for surveillance of alcohol consumption (49%), mental illness (46%), healthy eating (37%), and lifestyle behaviors (35%). In terms of geographic scale, most respondents supported citywide surveillance (85%) with markedly lower levels of support for smaller (less anonymous) geographic scales covered by specific locations. Wastewater surveillance does not receive the public pushback that other COVID-19-related health system actors have witnessed. Instead, the public supports the expansion of wastewater surveillance as a standard to complement public health tools in other areas of health protection., Competing Interests: The authors declare there is no conflict., (© 2024 The Authors This is an Open Access article distributed under the terms of the Creative Commons Attribution Licence (CC BY 4.0), which permits copying, adaptation and redistribution, provided the original work is properly cited (http://creativecommons.org/licenses/by/4.0/).)

Wastewater-based epidemiology (WBE) has emerged as a valuable tool for COVID-19 monitoring, especially as the frequency of clinical testing diminishes. Beyond COronaVIrus Disease 19 (COVID-19), the tool's versatility extends to addressing various public health concerns, including antibiotic resistance and drug consumption. However, the complexity of sewage systems introduces noise when measuring chemical tracer concentrations, potentially compromising their applicability for modeling. In our study, we detail the approach adopted to determine the concentration of severe acute respiratory syndrome coronavirus 2 (SARS CoV-2) ribonucleiec acid (RNA) in wastewater from the Ponte a Niccheri wastewater treatment plant in Tuscany (Italy), with a sample size of N = 13,935 inhabitants. The unique characteristics of this wastewater system, including mandatory pretreatment in septic tanks with extended retention times, the presence of a hospital for COVID-19 patients, and mixed sewage networks, posed additional challenges. Nevertheless, our results highlight a robust and significant correlation between our measurements and the number of infections within the wastewater treatment plant's catchment area at the time of sampling. A simple linear model also shows promising results in estimating the number of infected people within the area., Competing Interests: The authors declare there is no conflict., (© 2024 The Authors This is an Open Access article distributed under the terms of the Creative Commons Attribution Licence (CC BY 4.0), which permits copying, adaptation and redistribution, provided the original work is properly cited (http://creativecommons.org/licenses/by/4.0/).)

The present investigation focuses on the identification of popular PhACs in roots, leaves and rice grains, which are cultivated in soil irrigated with waters and wastewater. The present study reveals the presence of PhACs in rice grains from different brands which are available in the current market, which has thus motivated these experiments. The rice plants were cultivated in garden containers and irrigated with three different water sources. All PhAC compounds were recovered within an 89-111 % range using the extraction technique, reproducibility, and sensitivity (LOQ <25 µg/g). Further, PhAC compounds were identified using liquid chromatography quadrupole time-of-flight mass spectrometry (LC-QqTOF-MS). Interestingly, several PhAC compounds were detected in rice grains, aligning with hypotheses and findings from published literature. A total of ten (10) PhACs were found in the root, leaf, and rice grain of the 20 popular PhACs that were targeted. The annual exposure and medical dose equivalent for individual PhACs was negligible. According to our knowledge, this study is the first to show the accumulation of several categories (cocktail) of PhACs in rice grains and show the approximate human health risk assessment by its consumption. The study's results provide valuable insights for researchers, policymakers, and agricultural practitioners working on sustainable agriculture and public health., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)

This paper presents the results of a research aimed at establishing a novel method for the detection of primary and secondary micro- and nanoplastics (MNPs), by using the fluorescence properties of the dye Nile Red-n-heptane (NR-H). The method has been applied to the detection of laboratory degraded polymers (Polystyrene, PS and Polyethylene Terephthalate, PET) as well as traceable latex microspheres in aqueous environments, showing a remarkable detection capacity and avoiding the prior extraction or processing of MNPs in natural samples, with significant time savings compared to conventional methods. The study has been carried out on various types of water, including samples from wastewater treatment plants, boreholes, seawater and synthesized seawater. The effectiveness of the staining process was evaluated by scanning electron microscopy (SEM), dynamic light scattering (DLS) and optical microscopy. As a result, a novel standardizable protocol for the rapid detection of MNPs has been established, with the potential to improve environmental protection through fast in-situ detection and identification of plastic contaminants. The limitations of the protocol in the quantification of MNPs have also been identified and further studies are proposed to overcome these limitations., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper. IFTS-Project research reports financial support and administrative support were provided by Nouvelle-Aquitaine Regional Council. No conflict of interest to report. If there are other authors, they declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

The study of dissolved organic matter (DOM) presents a significant challenge for environmental analyses and the monitoring of wastewater treatment plants (WWTPs). This is particularly true for the tracking of recalcitrant to biodegradation dissolved organic matter (rDOM) compounds, which is generated during the thermal pretreatment of sludge. This study aims to develop analytical and chemometric methods to differentiate melanoidins from humic acids (HAs), two components of rDOM that require monitoring at various stages of wastewater treatment processes due to their distinct biological effects. The developed method implements the separation of macromolecules through ultra-high-performance liquid chromatography size-exclusion chromatography (U-HPLC SEC) followed by online UV and fluorescence detection. UV detection was performed at 210, 254, and 280 nm, and fluorescence detection at six excitation/emission pairs: 230/355 nm, 270/355 nm, 240/440 nm, 270/500 nm, 330/425 nm, and 390/500 nm. Chromatograms obtained for each sample from these nine detection modes were integrated and separated into four molecular fractions: >40 kDa, 20-40 kDa, 10-20 kDa, and <10 kDa. To enhance analytical resolution and normalize the data, ratios were calculated from the areas of chromatographic peaks obtained for each detection mode. The results demonstrate the utility of these ratios in discriminating samples composed of HAs, melanoidins, and their mixtures, through principal component analysis (PCA). Low molecular weight fractions were found to be specific to melanoidins, while high molecular weight fractions were characteristic of HAs. For the detection modes specific to melanoidins, UV absorbance at 210, 254, and 280 nm were predominantly present in the numerators, with tryptophan-like fluorescence emissions in the denominators. Conversely, fluorescence emissions largely represented both numerators and denominators for HAs. This online method also enables the discrimination of pseudo-melanoidins, compounds revealing a nitrogen deficiency in their chemical structures., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 The Authors. Published by Elsevier Ltd.. All rights reserved.)