Suspect Screening Research Articles

Occurrence and Contamination Profile of Legacy and Emerging Per- and Polyfluoroalkyl Substances (Pfas) in Belgian Wastewater Using Target, Suspect and Non-Target Screening Approaches

Occurrence and Contamination Profile of Legacy and Emerging Per- and Polyfluoroalkyl Substances (Pfas) in Belgian Wastewater Using Target, Suspect and Non-Target Screening Approaches

Enhancing Spectral Quality in Complex Environmental Matrices: Supporting Suspect and Non-Target Screening in Zebra Mussels with Ion Mobility

Enhancing Spectral Quality in Complex Environmental Matrices: Supporting Suspect and Non-Target Screening in Zebra Mussels with Ion Mobility

Enhanced Database Creation with in Silico Workflows for Suspect Screening of Unknown Pesticide Transformation Products in Environmental Samples by Uhplc-Hrms

Enhanced Database Creation with in Silico Workflows for Suspect Screening of Unknown Pesticide Transformation Products in Environmental Samples by Uhplc-Hrms

High Resolution Mass Spectrometric Suspect Screening, Wide-Scope Target Analysis of Emerging Contaminants and Determination of Legacy Pollutants in Adult Western Black-Tailed Godwit Limosa Limosa Limosa in the Netherlands – a Pilot Study

High Resolution Mass Spectrometric Suspect Screening, Wide-Scope Target Analysis of Emerging Contaminants and Determination of Legacy Pollutants in Adult Western Black-Tailed Godwit Limosa Limosa Limosa in the Netherlands – a Pilot Study

The Use of Gas Chromatography – High Resolution Mass Spectrometry for Suspect Screening and Non-Targeted Analysis of Polyfluorinated Alkyl Substances (PFAS)

The Use of Gas Chromatography – High Resolution Mass Spectrometry for Suspect Screening and Non-Targeted Analysis of Polyfluorinated Alkyl Substances (PFAS)

Target and Suspect Screening of (New) Psychoactive Substances by Lc-Hrms in South Korea

Target and Suspect Screening of (New) Psychoactive Substances by Lc-Hrms in South Korea

Comprehensive Investigation of Persistent and Mobile Chemicals and Per- and Polyfluoroalkyl Substances in Urine of Flemish Adolescents Using a Suspect Screening Approach

Comprehensive Investigation of Persistent and Mobile Chemicals and Per- and Polyfluoroalkyl Substances in Urine of Flemish Adolescents Using a Suspect Screening Approach

Target Analysis and Suspect Screening of Per- and Poly-Fluoroalkyl Substances in Paired Samples of Maternal Serum, Umbilical Cord Serum, and Placenta Near Fluorochemical Plants in Fuxin, China

Target Analysis and Suspect Screening of Per- and Poly-Fluoroalkyl Substances in Paired Samples of Maternal Serum, Umbilical Cord Serum, and Placenta Near Fluorochemical Plants in Fuxin, China

Target and Suspect Screening of Pesticide Residues in Soil Samples from Peach Orchards Using Liquid Chromatography Quadrupole Time-of-Flight Mass Spectrometry

Target and Suspect Screening of Pesticide Residues in Soil Samples from Peach Orchards Using Liquid Chromatography Quadrupole Time-of-Flight Mass Spectrometry

Target and Suspect Screening of 4,777 Per- and Polyfluoroalkyl Substances (Pfas) in River Water, Wastewater, Groundwater and Biota Samples in the Danube River Basin

Target and Suspect Screening of 4,777 Per- and Polyfluoroalkyl Substances (Pfas) in River Water, Wastewater, Groundwater and Biota Samples in the Danube River Basin

Target and Suspect Screening of Urinary Biomarkers for Current-use Pesticides: Application of a Simple Extraction Method.

Pesticide residues pose a great threat to human health. Biomonitoring with urine samples has often been used to assess pesticide exposure to humans, and identifying appropriate biomarkers is a premise of success. Current-use pesticides (CUPs) including neonicotinoids tend to be transformed in an organism, and thus the biomonitoring studies focusing on parent compounds alone may underestimate their risk. It is imperative to develop effective methods to analyze CUPs and their metabolites simultaneously and to identify viable metabolites as urinary biomarkers. For analyzing xenobiotics in urine, we optimized CH3 COCH3 -MgSO4 extraction coupled with a high-performance liquid chromatography-tandem mass spectrometry detection method. The method had sensitive method detection limits (0.11-1.39 ng/ml), low matrix effects, and satisfactory recovery and precision (49.4% ± 7.2%-99.8% ± 17.8%) for neonicotinoids and their metabolites. Application of the method for real samples showed that children living in rural areas in South China were ubiquitously exposed to CUPs, including neonicotinoids, fipronil, and chlorpyrifos, and urinary residues were mainly in the form of metabolites. Suitable biomarkers were identified for individual neonicotinoids, including imidacloprid-olefin and imidacloprid-guanidine for imidacloprid, acetamiprid-N-desmethyl for acetamiprid, thiacloprid-amide for thiacloprid, and N-desmethyl-thiamethoxam and thiamethoxam for thiamethoxam. Three metabolites were mainly reported in urine samples, including imidacloprid-urea, thiacloprid-amide, and N-desmethyl-thiamethoxam. In addition, the method was also applied for suspect screening, and an additional metabolite (clothianidin-desmethyl-nitrosoguanidine) was identified, showing its potential application in suspect analysis. Environ Toxicol Chem 2022;41:73-80. © 2021 SETAC.

Suspect screening of antimicrobial agents transformation products in environmental samples development of LC-QTrap method running in pseudo MRM transitions

The aim of the work was to develop a new HPLC-MS/MS method that allows for the simultaneous detection of antimicrobials agents (targeted analysis) and their transformation products (non-targeted analysis), which enabled the elucidation of their transformation pathways in the environment. Targeted analysis was performed for 16 selected antimicrobials agents (AMs) in wastewater collected at different stages of the treatment process and river water from sections before and after wastewater discharge. The samples were collected in the Łyna sewage treatment plant (Olsztyn, Poland) in three measuring periods at different seasons. Analytes were selected from tetracyclines, fluoroquinolones, β-lactams, macrolides, glycopeptides, lincosamides and synthetic antibiotics.As a part of the targeted analysis, 13 AMs were detected in wastewater samples, and 7 of them in river water samples. However, their presence and concentrations were closely related to the type of the sample and the season in which the sample was taken. The highest concentrations of AMs were detected in samples collected in September (max. 1643.7 ng L−1 TRI), while the lowest AMs concentrations were found in samples collected in June (max. 136.1 ng L−1 CLR). The total content of AMs in untreated wastewater was in the range of 1.42–1644 ng L−1, while in the river water was for upstream 1.22–48.73 ng L−1 and for downstream 2.24–149 ng L−1. In the non-target analysis, 33 degradation products of the selected AMs were identified, and the transformation pathways of their degradation were speculated. In the course of the research, it was found that as a result of the processes taking place in wastewater treatment plant, the parent substances are transformed into a number of stable transformation products. Transformation products resulted from hydroxylation, ring opening, oxidation, methylation or demethylation, carboxylation, or cleavage of the CN bond of the parent AMs.

Suspect, non-target and target screening of pharmaceuticals and personal care products (PPCPs) in a drinking water system

Drinking water quality and safety are very important in protecting human health. Chemical contaminants in drinking water system have become an increasing concern. Our knowledge about what chemicals are present in drinking water is still limited. Here we screened chemicals of emerging concern in a conventional drinking water system based on suspect, non-target screening and target analysis, and assessed their variations in different seasons and different treatment units. Overall, 720 chemicals were identified with HRMS databases from the suspect and non-target screening and 48 chemicals in five categories were further confirmed with the high confidence level, with predominance of pharmaceuticals and personal care products (PPCPs) and pesticides. Four compounds are newly found in aquatic environment with no literature or chemical occurrence data record. Temporal variations and variable removals were observed for these chemicals in the system. Target analysis of 110 PPCPs showed detection of 21, 19 and 22 compounds in the drinking water treatment plant with a concentration range of 0.11–844 ng/L in the three seasons, but only 8, 9 and 15 compounds detected in tap water (0.16–32.5 ng/L). The variations of the detected chemicals were less obvious in tap water, with most having concentrations below 2 ng/L. The results indicated efficient removal for most PPCPs in the drinking water system. The findings from this study demonstrated the strong capability of combined non-target screening and target analysis in identifying and assessing various organic chemicals in drinking water system.

Suspect and non-target screening of chemicals in clothing textiles by reversed-phase liquid chromatography/hybrid quadrupole-Orbitrap mass spectrometry

The global manufacturing of clothing is usually composed of multistep processes, which include a large number of chemicals. However, there is generally no information regarding the chemical content remaining in the finished clothes. Clothes in close and prolonged skin contact may thus be a significant source of daily human exposure to hazardous compounds depending on their ability to migrate from the textiles and be absorbed by the skin. In the present study, twenty-four imported garments on the Swedish market were investigated with respect to their content of organic compounds, using a screening workflow. Reversed-phase liquid chromatography coupled to electrospray ionization/high-resolution mass spectrometry was used for both suspect and non-target screening. The most frequently detected compound was benzothiazole followed by quinoline. Nitroanilines with suspected mutagenic and possible skin sensitization properties, and quinoline, a carcinogenic compound, were among the compounds occurring at the highest concentrations. In some garments, the level of quinoline was estimated to be close to or higher than 50,000 ng/g, the limit set by the REACH regulation. Other detected compounds were acridine, benzotriazoles, benzothiazoles, phthalates, nitrophenols, and organophosphates. Several of the identified compounds have logP and molecular weight values enabling skin uptake. This pilot study indicates which chemicals and compound classes should be prioritized for future quantitative surveys and control of the chemical content in clothing as well as research on skin transfer, skin absorption, and systemic exposure. The results also show that the current control and prevention from chemicals in imported garments on the Swedish market is insufficient.Graphical abstract

Coupling Suspect and Nontarget Screening with Mass Balance Modeling to Characterize Organic Micropollutants in the Onondaga Lake–Three Rivers System

Characterizing the occurrence, sources, and fate of organic micropollutants (OMPs) in lake–river systems serves as an important foundation for constraining the potential impacts of OMPs on the ecosystem functions of these critical landscape features. In this work, we combined suspect and nontarget screening with mass balance modeling to investigate OMP contamination in the Onondaga Lake–Three Rivers system of New York. Suspect and nontarget screening enabled by liquid chromatography–high-resolution mass spectrometry led to the confirmation and quantification of 105 OMPs in water samples collected throughout the lake–river system, which were grouped by their concentration patterns into wastewater-derived and mixed-source clusters via hierarchical cluster analysis. Four of these OMPs (i.e., galaxolidone, diphenylphosphinic acid, N-butylbenzenesulfonamide, and triisopropanolamine) were prioritized and identified by nontarget screening based on their characteristic vertical distribution patterns during thermal stratification in Onondaga Lake. Mass balance modeling performed using the concentration and discharge data highlighted the export of OMPs from Onondaga Lake to the Three Rivers as a major contributor to the OMP budget in this lake–river system. Overall, this work demonstrated the utility of an integrated screening and modeling framework that can be adapted for OMP characterization, fate assessment, and load apportionment in similar surface water systems.

Vertical profile and assessment of soil pollution from a typical coking plant by suspect screening and non-target screening using GC/QTOF-MS

A comprehensive workflow for suspect screening and non-target screening with gas chromatography coupled with quadrupole time-of-flight mass spectrometry (GC/QTOF-MS) was used to characterize the pollution characteristics of soil samples in a typical coking plant in China. Suspect screening confirmed 57 chemicals including PAHs, alkyl PAHs, and phthalates contained in high-resolution personal compound database and library (PCDL). Non-target screening detected 88 chemicals from soil samples in the NIST 17 library. A total of 122 chemicals were screened in soil samples, and many of them were of emerging concern. Their presence in the soil obtained from coking operations has been underestimated, such as the oxygenated PAHs (naphtho[2,1-b]furan and 9H-fluoren-9-one), and the alkyl biphenyls compounds (4,4′-dimethylbiphenyl, 3,3′-dimethylbiphenyl, 4-methyl-1,1′-biphenyl and 2,2′,5,5′-tetramethyl-1,1′-biphenyl). Toxicity assays by luminescent bacteria proved that the extracts from soil samples at different depths showed varying toxicity to V. qinghaiensis sp.-Q67. Soil extracts from a depth of 20–40 cm exhibited the greatest toxicity to luminescent bacteria compared with the other six-layered soil samples, which was correlated with the number of detectable pollutants and total organic carbon content. This study provided a screening method for suspect and non-target contaminants in urban industrial soil sites, which was important in identifying localized contamination sources.

Human metabolism and urinary excretion of seven neonicotinoids and neonicotinoid-like compounds after controlled oral dosages

Few human data on exposure and toxicity are available on neonicotinoids and neonicotinoid-like compounds (NNIs), an important group of insecticides worldwide. Specifically, exposure assessment of humans by biomonitoring remains a challenge due to the lack of appropriate biomarkers. We investigated the human metabolism and metabolite excretion in urine of acetamiprid (ACE), clothianidin (CLO), flupyradifurone (FLUP), imidacloprid (IMI), sulfoxaflor (SULF), thiacloprid (THIAC) and thiamethoxam (THIAM) after single oral dosages at the currently acceptable daily intake levels of the European Food Safety Authority. Consecutive post-dose urine samples were collected up to 48 h. Suspect screening of tentative metabolites was carried out by liquid chromatography–high-resolution mass spectrometry. Screening hits were identified based on their accurate mass, isotope signal masses and ratios, product ion spectra, and excretion kinetics. We found, with the exception of SULF, extensive metabolization of NNIs to specific metabolites which were excreted next to the parent compounds. Overall, 24 metabolites were detected with signal intensities indicative of high metabolic relevance. Phase-I metabolites were predominantly derived by mono-oxidation (such as hydroxy-FLUP, -IMI, and -THIAC) and by oxidative N-desalkylation (such as N-desdifluoroethyl-FLUP and N-desmethyl-ACE, -CLO and -THIAM). IMI-olefin, obtained by dehydration of hydroxylated IMI, was identified as a major metabolite of IMI. SULF was excreted unchanged in urine. Previously reported metabolites of NNIs such as 6-chloronicotinic acid or 2-chlorothiazole-4-carboxylic acid and their glycine derivatives were detected either at low signal intensities or not at all and seem less relevant for human biomonitoring. Our highly controlled approach provides specific insight into the human metabolism of NNIs and suggests suitable biomarkers for future exposure assessment at environmentally relevant exposures.

Identifying Citric Acid Esters, a Class of Phthalate Substitute Plasticizers, in Indoor Dust via an Integrated Target, Suspect, and Characteristic Fragment-Dependent Screening Strategy.

Citrate acid esters (CAEs) have been proposed as a class of phthalate substitute plasticizers; however, information on their occurrence in indoor environments is rare. By using liquid chromatography coupled with a quadrupole-Orbitrap mass spectrometer, we developed an integrated strategy that can be applied for target, suspect, and characteristic fragment-dependent screening of CAEs. In n = 50 indoor dust samples collected from Nanjing City (China), three CAEs, namely, acetyl tributyl citrate (ATBC; mean: 412,000 ng/g), tributyl citrate (TBC, 11,600 ng/g), and triethyl citrate (TEC, 10,900 ng/g), exhibited the greatest contamination levels. Total concentrations of CAEs (∑8CAEs) were statistically significantly (p < 0.01) greater than those of common organophosphate triesters (OPTEs), a class of ubiquitous contaminants in dust. Suspect and characteristic fragment-dependent screening (m/z 111.0078 ([C5H3O3]+) and m/z 129.0181 ([C5H5O4]+)) of CAEs were further conducted for the same batch of samples. We tentatively identified six novel CAEs, and the most frequent and abundant CAE was fully identified as tributyl aconitate (TBA). Statistically significant correlation relationships were observed on dust levels between TBA vs ATBC (r = 0.650; p < 0.01) and TBA vs TBC (r = 0.384; p < 0.01), suggesting their similar sources in dust samples.

Discovering pesticides and their TPs in Luxembourg waters using open cheminformatics approaches

The diversity of hundreds of thousands of potential organic pollutants and the lack of (publicly available) information about many of them is a huge challenge for environmental sciences, engineering, and regulation. Suspect screening based on high-resolution liquid chromatography-mass spectrometry (LC-HRMS) has enormous potential to help characterize the presence of these chemicals in our environment, enabling the detection of known and newly emerging pollutants, as well as their potential transformation products (TPs). Here, suspect list creation (focusing on pesticides relevant for Luxembourg, incorporating data sources in 4 languages) was coupled to an automated retrieval of related TPs from PubChem based on high confidence suspect hits, to screen for pesticides and their TPs in Luxembourgish river samples. A computational workflow was established to combine LC-HRMS analysis and pre-screening of the suspects (including automated quality control steps), with spectral annotation to determine which pesticides and, in a second step, their related TPs may be present in the samples. The data analysis with Shinyscreen (https://gitlab.lcsb.uni.lu/eci/shinyscreen/), an open source software developed in house, coupled with custom-made scripts, revealed the presence of 162 potential pesticide masses and 96 potential TP masses in the samples. Further identification of these mass matches was performed using the open source approach MetFrag (https://msbi.ipb-halle.de/MetFrag/). Eventual target analysis of 36 suspects resulted in 31 pesticides and TPs confirmed at Level-1 (highest confidence), and five pesticides and TPs not confirmed due to different retention times. Spatio-temporal analysis of the results showed that TPs and pesticides followed similar trends, with a maximum number of potential detections in July. The highest detections were in the rivers Alzette and Mess and the lowest in the Sûre and Eisch. This study (a) added pesticides, classification information and related TPs into the open domain, (b) developed automated open source retrieval methods - both enhancing FAIRness (Findability, Accessibility, Interoperability and Reusability) of the data and methods; and (c) will directly support “L’Administration de la Gestion de l’Eau” on further monitoring steps in Luxembourg.

Large-Scale Implementation and Flaw Investigation of Human Serum Suspect Screening Analysis for Industrial Chemicals.

Non-targeted analysis (NTA), including both suspect screening analysis (SSA) and unknown compound analysis, has gained increasing popularity in various fields for its capability in identifying new compounds of interests. Current major challenges for NTA SSA are that (1) tremendous effort and resources are needed for large-scale identification and confirmation of suspect chemicals and (2) suspect chemicals generally show low matching rates during identification and confirmation processes. To narrow the gap between these challenges and smooth implementation of NTA SSA methodology in the biomonitoring field, we present a thorough SSA workflow for the large-scale screen, identification, and confirmation of industrial chemicals that may pose adverse health effects in pregnant women and newborns. The workflow was established in a study of 30 paired maternal and umbilical cord serum samples collected at delivery in the San Francisco Bay area. By analyzing LC-HRMS and MS/MS data, together with the assistance of a combination of resources including online MS/MS spectra libraries, online in silico fragmentation tools, and the EPA CompTox Chemicals Dashboard, we confirmed the identities of 17 chemicals, among which monoethylhexyl phthalate, 4-nitrophenol, tridecanedioic acid, and octadecanedioic acid are especially interesting due to possible toxicities and their high-volume use in industrial manufacturing. Similar to other previous studies in the SSA field, the suspect compounds show relatively low MS/MS identification (16%) and standard confirmation (8%) rates. Therefore, we also investigated origins of false positive features and unidentifiable suspected features, as well as technical obstacles encountered during the confirmation process, which would promote a better understanding of the flaw of low confirmation rate and encourage gaining more effective tools for tackling this issue in NTA SSA.