Analytical Chemistry, Water Science and Technology, Environmental Chemistry, Environmental Science
13
Scopus Publications
Scopus Publications
Comprehensive HRMS-screening for persistent, mobile, and toxic compounds in first flush urban stormwater Sergio Santana-Viera, Francesc Labad, Marina G. Pintado-Herrera, Nicola Montemurro, Marc Teixidó, Pablo A. Lara-Martín, Sandra Pérez Npj Clean Water, 2025 Water scarcity drives water-stressed regions to make use of all available resources. Consequently, urban stormwater is gaining recognition as a valuable resource, for instance to replenish aquifers; thus, enhancing water supply. However, it carries contaminants that could limit its potential uses, highlighting those recently categorized as persistent, mobile, and toxic (PMT) compounds. In order to conduct broad screening for the presence of PMT compounds in stormwater first-flush samples and rainwater, two instruments based on Gas and Liquid Chromatography coupled to Quadrupole-Time-of-Flight Mass Spectrometry were used, and both suspect and target screening were performed. After prioritization 42 PMTs were detected, of which 24 PMTs were quantified. The results showed that 66% of the quantified PMTs were present in more than 50% of the samples, with average concentrations ranging from 2 ng L -1 to 2.78 µg L -1 . Of the target PMTs, 11 were quantified for the first time in runoff samples.
Qualitative and quantitative analysis of highly-polar contaminants in Atlanta urban water Francesc Labad, Sandra Pérez Analytica Chimica Acta, 2025 Highly polar substances have fallen from the scope of investigations due to this lack of accumulation into organic materials and the analytical difficulty they present using “traditional” techniques. This study presents an integrated analytical approach combining liquid chromatography (LC) and travelling-wave ion mobility spectrometry (TWIMS) coupled with high-resolution mass spectrometry (HRMS) for the separation, detection, and quantification of 45 challenging contaminants in urban water matrices. The targeted analytes, including 41 very mobile compounds and 37 highly polar substances (log D ow < 0), represent compounds that are often poorly retained under conventional reversed-phase and HILIC LC conditions. TWIMS was used to determine the CCS of 33 small organic molecules (120–500 Da). A ΔCCS threshold of ≥0.5% was identified as sufficient for proper separation on second-generation IMS instruments (resolving power >300 Rp). In cases where LC provided inadequate retention, TWIMS proved to be an effective complementary technique by exploiting differences in molecular size, shape, and charge to resolve compounds based on their collision cross-section (CCS) values. Surface water samples from the Chattahoochee River and tap water from Midtown Atlanta (USA) were analyzed, revealing that over 50% of the targeted contaminants were detected in at least one matrix. Notably, compounds such as naphthalene-1-sulfonic acid, nicotine, and several per- and poly-fluoroalkyl substances (PFAS) were consistently observed, highlighting their ubiquitous occurrence in urban water impacted by industrial activities and heavy traffic. The methodology employed not only improved the resolution and identification of small, highly polar molecules but also provided robust quantitative data essential for environmental monitoring and risk assessment. This approach underscores the potential of IMS as a valuable complementary tool to traditional LC-MS workflows in complex environmental analyses. Additionally, the data presented regarding the presence of highly polar substances in urban water matrices should inform stakeholders and implement preventive strategies. • Determination of 33 CCS compounds, 30 of them for the first time. • TWIMS provided reliable CCS values when compared to DTIMS. • The functional groups of the target analytes revealed a trend in their CCS values. • IM was able to separate compounds poorly retained in LC. • Several organic compounds in an urban river of Atlanta were determined.
Identifying sources and environmental risks of emerging mobile organic pollutants in the urban groundwater of Barcelona (Spain) Francesc Labad, Anna Jurado, Laura Scheiber, Marc Teixidó, Enric Vázquez-Suñé, Sandra Pérez Environmental Chemistry and Ecotoxicology, 2025 Groundwater is a vital yet vulnerable resource, subject to contamination from recharge sources and water system leaks by organic pollutants, including personal care products, pharmaceuticals, sweeteners, and industrial chemicals. Despite recent European regulatory progress with the 2022 amendments to Directive 2006/118/EC, many mobile pollutants remain unregulated. This study identified 129 organic compounds, including very mobile pollutants (vM) derived from pharmaceuticals, industrial chemicals, and tyre wear, across 197 urban water samples from Barcelona city. They comprised stormwater, surface water, untreated sewage, nine groundwater samples influenced by river infiltration, rainwater, sustainable urban drainage systems infiltrates, and 32 other groundwater samples. The results showed higher detection frequencies and concentrations of highly polar pollutants (log Dow < 0). Most of the 129 detected compounds were found across all water types, with 41 occurring in stormwater, groundwater, surface water, and sewage, highlighting their widespread presence in urban waters. The study also assessed pollution sources, finding that sewage system leaks and surface water were the main contributors to groundwater contamination, with runoff-associated contaminants such as industrial compounds becoming more prominent as distance from the river increased. The environmental risk assessment highlighted significant risks from pharmaceuticals like atorvastatin, ciprofloxacin, and iopamidol, as well as melamine, showing moderate environmental risk. These findings emphasize the need for continued monitoring to better understand the threats posed by these pollutants to groundwater quality.
LC–MS analysis of polar and highly polar organic pollutants in Barcelona urban groundwater using orthogonal LC separation modes Francesc Labad, Sandra Pérez Environmental Science and Pollution Research, 2024 Groundwater samples may contain thousands of organic pollutants from infiltration of surface water, sewer leakages, and to a minor extent from public water supply network losses. Polar (0 < log D < − 2.0) and very polar substances (log D < − 2.0) have been largely beyond the scope of applied analytical methodologies in environmental monitoring because of challenges related to their extraction from the sample and subsequent chromatographic separation. In this study, we developed an analytical workflow for 96 pollutants covering a broad polarity range, including pharmaceuticals, industrial chemicals, and artificial sweeteners, potentially seeping through the soil in urban areas. The Besos aquifer located at the Northern-eastern edge of the city of Barcelona was chosen as a study area due to the deterioration of the quality of the aquifers over the past years and the proven presence of numerous pollutants. The methodology consisted of vacuum-assisted evaporation (VAE) followed by chromatographic separation of the sample on two columns with orthogonal retention mechanisms, namely, an HSS T3 column (modified C18) and a BEH amide column (HILIC). The analytes were detected by high-resolution mass spectrometry on a Q Exactive Orbitrap system in data-independent acquisition mode. Taking into consideration the retention as well as the peak shape, a Quality Score (QS) was assigned for each analyte to evaluate the quality of each chromatographic peak of each compound. While 67 compounds, including 19 polar and 48 moderately polar, were satisfactorily retained on an HSS T3, 29 compounds, including 14 highly polar, 14 polar, and one moderately polar, were analyzed in the BEH amide column. The optimized methodology was applied for the analysis of 89 out of 96 validated contaminants with satisfactory recoveries in samples collected from seven wells, providing low LODs (0.02 to 0.45 ng L−1) and LOQs (0.06 to 1.34 ng L−1). A number of highly polar and polar compounds not previously reported to occur in GW, including artificial sweeteners, pharmaceuticals, and industrial chemicals, were detected at concentrations as high as few $$\\mu$$ μ g L−1.
HRMS-Targeted-DIA methodology for quantification of wastewater-borne pollutants in surface water Olga Gómez-Navarro, Francesc Labad, Diana P Manjarrés-López, Sandra Pérez, Nicola Montemurro Methodsx, 2023 A robust method was developed for the quantification of popular and highly occurrence contaminants of emerging concern from wastewater treatment plant effluents and is explained in detail. A homemade multi-layered and multi-sorbent solid phase extraction (SPE) cartridge was used to cover the wide range of polarities of the selected contaminants. A non-discriminant elution protocol was also applied. Liquid chromatography coupled to a high-resolution mass spectrometer (HRMS) Q-Exactive Orbitrap system was used for the separation and detection of the contaminants. A targeted data independent acquisition (DIA) mode with an inclusion list with the exact mass, retention time window and collision energy was tried for the first time obtaining good sensitivity, selectivity and high quality MS2 product ions.•116 compounds of a wide-scope of polarities and physic-chemical properties were validated using a surface water pool matrix.•SPE followed by LC HRMS with a targeted DIA was used for the method validation at three concentration levels 5, 50, 500 μg l-1 in extract.•Good recoveries were obtained between 70 and 120% for the majority of the selected contaminants. Matrix effect, precision, and linearity were also evaluated and results proved the suitability for the method application.
Occurrence, data-based modelling, and risk assessment of emerging contaminants in an alluvial aquifer polluted by river recharge Francesc Labad, Antoni Ginebreda, Rotman Criollo, Enric Vázquez-Suñé, Sandra Pérez, Anna Jurado Environmental Pollution, 2023 This research presents the occurrence and fate of 121 contaminants of emerging concern (CECs) in an urban aquifer polluted by river recharge through a data-base modelling. Afterwards, risk quotients (RQs) are computed to determine the risk posed by CECs to human health. To this end, groundwater and river water samples were collected in four campaigns conducted from February to May 2021. Results show that 46 CECs are ubiquitous in groundwater and their concentrations vary several orders of magnitude, ranging from below the limit of quantification to 44.5·103 ng/L for iopamidol. Transformation products (TPs) are usually detected at lower concentrations than those of the parent substances but there are some exceptions (i.e., fipronil sulphide, fipronil sulfone and O-desmethylvenlafaxine). River concentrations are higher than those detected in groundwater for some CECs, indicating the occurrence of natural attenuation processes when river water infiltrates the aquifer. A data-based advection-reaction modelling is proposed and tested for ca. 40 substances with detection frequencies higher than 90%. It provides useful quantitative information regarding the dynamic behaviour of the variables monitored, expressed in terms of characteristic length, entropy and synchronized state contribution. Finally, risk quotients (RQs) are used to assess the human health risk posed by the ubiquitous CECs in groundwater. Most CECs do not pose any risk to the different life stages considered, as the RQs evaluated are lower than 0.01. However, the pharmaceuticals valsartan and its TP valsartan acid show RQs higher than 1, indicating that these substances might be harmful to human beings.
ASSET project: assessing sustainable urban drainage system (SUDS) efficiency to reduce urban runoff water contamination Laura Scheiber, Marc Teixidó, Rotman Criollo, Francesc Labad, Enric Vázquez-Suñé, María Izquierdo, María José Chesa Marro, Daniel de Castro Advances in Geosciences, 2022 Increase of population in the current climate change scenario requires to ensure the quality of groundwater available as well as to control possible incomes of pollution into the subsurface system. The objective of this work was to evaluate the current quality of groundwater and the risk of infiltration of surface contaminants into the aquifers customizing the DRASTIC method including potential flood areas and areas with high risk of surface pollution. Hydrogeological, hydrochemical and isotopic data compiled and measured show the aquifer behavior and the main attenuation and degradation of contaminants. The vulnerability to contamination of Barcelona aquifers by direct surface contaminants is relatively low considering flood areas and traffic. However, there is a relevant area where this risk is relatively high. Nevertheless, it is required further analyses considering the drainage network of the city including as well the geometry of Sustainable Urban Drainage Systems (SUDS) already installed. The knowledge of the aquifer hydrogeological characteristics and its quality together with the identification of vulnerable to contamination areas may lead to improve the installation of SUDS, reducing the input of contaminants through these infrastructures. The implementation of this methodology aims to facilitate water users and urban managers to control their potential negative effects on the receiving water body. In addition, the outcomes of its application may be used to optimize the groundwater management in the city.
