Ailette Prieto

Universidad del País Vasco / Euskal Herriko Unibertsitatea | UPV/EHU · Analytical Chemistry

This investigation deals with how temperature influences oil toxicity, alone or combined with dispersant (D). Larval lengthening, abnormalities, developmental disruption, and genotoxicity were determined in sea urchin embryos for assessing toxicity of low-energy water accommodated fractions (LEWAF) of three oils (NNA crude oil, marine gas oil -MGO-...

Micropollutants monitoring in wastewater can serve as a picture of what is consuming society and how it can impact the aquatic environment. In this work, a suspect screening approach was used to detect the known and unknown contaminants in wastewater samples collected from two wastewater treatment plants (WWTPs) located in the Basque Country (Crisp...

The increasing number of contaminants in the environment has pushed water monitoring programs to find out the most hazardous known and unknown chemicals in the environment. Sample treatment-simplification methods and non-target screening approaches can help researchers to not overlook potential chemicals present in complex aqueous samples. In this...

An effect-directed analysis (EDA) approach was used to identify the compounds responsible for endocrine disruption in a hospital effluent (Basque Country). In order to facilitate the identification of the potentially toxic substances, a sample was collected using an automated onsite large volume solid phase extraction (LV-SPE) system. Then, it was...

In the present work, a target analysis method for simultaneously determining 24 diverse endocrine-disrupting compounds (EDCs) in urine (benzophenones, bisphenols, parabens, phthalates and antibacterials) was developed. The target analysis approach (including enzymatic hydrolysis, clean-up by solid-phase extraction and analysis by liquid chromatogra...

A combination of multitarget quantitative analysis and suspect screening was developed and applied to influent and effluent samples of two wastewater treatment plants (WWTPs) located in the Basque Country: Galindo and Crispijana, responsibles for the wastewater treatment of the metropolitan area of Bilbao (approximately 1 million inhabitants) and V...

Wastewater treatment plants (WWTPs) are one of the major secondary sources of contaminants of emerging concern (CECs) to the environment, since conventional treatments implemented are not efficient enough for their complete removal. The objective of the present work was the analysis of the efficiency of a new wastewater secondary treatment based on...

Perfluorinated alkyl substances (PFASs) are receiving an increasing worldwide attention due to their persistence, toxicity and widespread occurrence. This study provides the first wide-spread assessment of the occurrence and distribution of these contaminants in the Amazon River, the largest drainage basin in the world, including three different ab...

The massive use of antibiotics in cattle industry has led them to reach the food chain through the accumulation in plants and vegetables of frequent human consumption, among others. Consequently, major concern has arisen in the last decades regarding food safety and human health, not only due to the possible effects after ingestion of contaminated...

The COVID-19 pandemic spread rapidly worldwide in the year 2020, which was initially restrained by drastic mobility restrictions. In this work, we investigated the use of illicit drugs (amphetamine, methamphetamine, ecstasy, cocaine and cannabis), and licit substances of abuse (alcohol and tobacco) during the earlier months (March–July 2020) of the...

In this work, the formation and the chemical composition of Water Accommodated Fractions (WAFs) of Intermediate Fuel Oil 180, Naphthenic North Atlantic, and Marine Gas-Oil oils were studied at different temperatures (between 5 and 25 °C) with and without a dispersant (Finasol OSR52). In terms of composition, both the raw oils and the WAFs showed hi...

The city of Vitoria-Gasteiz was one of the probable first entrances of the SARS-CoV2 in Spain, one of the worst affected countries in the world during the first COVID 19 wave. Driven by the urgency of the situation, multiple drugs with antiviral activity were used off label. Sadly, most of these treatments were of little or no benefit and thus, the...

The interest in contaminants of emerging concern (CECs) has increased lately due to their continued emission and potential ecotoxicological hazards. Wastewater treatment plants (WWTPs) are generally not capable of eliminating them and are considered the main pathway for CECs to the aquatic environment. The number of CECs in WWTPs effluents is often...

Amphetamine (AMP), methamphetamine (MAMP) and 3,4-methylenedioxymethamphetamine (MDMA) occur in wastewater not only as a result of illicit consumption, but also, in some cases, from prescription drug use or by direct drug disposal into the sewage system. Enantiomeric profiling of these chiral drugs could give more insight into the origin of their o...

Perfluorinated alkyl substances (PFASs) are receiving an increasing worldwide attention due to their persistence, toxicity and widespread occurrence. These emerging contaminants have high water solubility and lower lipophilicity compared to legacy persistent organic pollutants, being their global fate still uncertain due to their chemical features....

The effects of urban, industrial and hospital wastewater discharges were evaluated on the occurrence of emerging contaminants (ECs) in three riverine basins impacted by wastewater treatment plants (WWTP) effluents. The objective was to identify ECs in water samples using different sampling techniques and targeted screening analysis with liquid chro...

Suspect and non-target screening (SNTS) techniques are arising as new analytical strategies useful to disentangle the environmental occurrence of the thousands of exogenous chemicals present in our ecosystems. The unbiased discovery of the wide number of substances present over environmental analysis needs to find a consensus with powerful technica...

Suspect screening techniques are able to determine a broader range of compounds than traditional target analysis. However, the performance of the suspect techniques relies on the procedures implemented for peak annotation and for this, the list of potential candidates is clearly a limiting factor. In order to study this effect on the number of comp...

The development of suspect or non-target screening methods to detect xenobiotics in biological fluids is essential to properly understand the exposome and assess its adverse health effects on humans. In order to fulfil that aim, the biomonitorization of human fluids is compulsory. However, these methods are not yet extensively developed, especially...

The migration of photoinitiators, phthalates and plasticizers from two paper and cardboard materials into food simulants (50% and 95% EtOH and Tenax) and foodstuffs (rice, cereals and milk powder) was studied. In the case of liquid simulants migration was observed to reach the equilibrium after 60 min and depended on the material type and the physi...

Debido a sus amplias aplicaciones, su estabilidad, presencia en el medioambiente y potencial toxicidad, los PFAS se han convertido en contaminantes emergentes presentes en una gran variedad de muestras acuosas. Dentro de este escenario, el principal objetivo del presente trabajo es la determinación de los niveles de PFAS en muestras de un transecto...

Sea urchin embryo assay was used to assess general toxicity at four wastewater treatment plant effluents of Biscay (Gorliz, Mungia, Gernika and Galindo) and, within the tested range, all the extracts showed embryo growth inhibition and skeleton malformation activities with EC50 values, in relative enrichment factor units, between 1.1-16.8 and 1.1-...

The development of multitarget and/or suspect screening methods for the analysis of xenobiotics in fish samples is compulsory due to the lack of works in the literature where a deep evaluation of the variables affecting extraction and clean-up steps is performed. The aim of the present work was to optimize and validate a multitarget (180 compounds)...

Municipal wastewater effluents contains a complex mixture of xenobiotic organic compounds (XOCs) originating from personal care products, pharmaceuticals, excreted hormones, household and industrial chemicals, among other emerging organic compounds. Within this context, the objective of the present work was the application of a multi-residue analys...

The analysis of the miriads of xenobiotics present in the environment stand for one of the more complex chalenges for scientists. Improvements of analytical instrumentation such as the development of different screening techniques in high resolution mass spectrometry points a promissing path for this purpose. The three main techniques include targe...

An effect-directed analysis protocol was developed and applied to to an hospital effluent (Biscay, Basque Country), one of the bigger hospitals in the Basque Country holding more than 800 beds and offering more than 13 specialities, using the sea urchin embryo test (SET) as toxicological in vivo bioassay. The objective was to identify compounds res...

Multi-target analysis of polar xenobiotics in fatty matrices such as milk is a challenge due to the high matrix effect that the co-extracted lipids and proteins cause during the detection step. The evolution of high-resolution tandem mass spectrometry renders the challenge to apply the methods developed and validated for a few hundreds of analytes...

This work describes the screening of twenty three per- and polyfluoroalkyl substances (PFASs) in twenty five paper and board (P/B) packaging materials and their migration to several food simulants (50 % ethanol, 95 % ethanol and Tenax®) at different conditions of time and temperature. A different migration pattern depending on the carbon chain leng...

An effect-directed analysis protocol was developed and applied to the Cruces hospital effluent (Barakaldo, Biscay, Basque Country) using the sea urchin embryo test (SET) as toxicological in vivo bioassay. The objective was to identify compounds responsible for the toxicity by combining state-of-the-art sampling, toxicology assays, fractionation and...

This work describes the analysis of both target and non-target compounds in paper and cardboard materials together with the characterization of their migration to Tenax® by means of liquid chromatography coupled to both low (LC-QqQ) and high resolution tandem mass spectrometry (LC-q-Orbitrap), respectively. To this aim, an entire analytical procedu...

This paper describes the stability study performed in seawater and seawater extracts (spiked at ~ 200 ng/L) for 23 emerging contaminants. Four different alternatives were tested at six different times (0, 3, 10, 17, 24 and 31 days): (i) seawater at 4 °C, (ii) mixed-mode solid-phase extraction cartridge (Bond Elute Plexa and Strata X-AW) stored at −...

The fate and distribution of new emerging contaminants and their unexpected effects in the environment are needed study topics, since most of the chemicals nowadays delivered in nature are unregulated and their effects are overlooked in many monitoring programs. These new chemicals include personal care products and pharmaceuticals (PCPPs) and cons...

The complexity of the occurrence and toxicity of emerging contaminants in aquatic environments is remarkable. On the one hand, the identification and quantification of unknown pollutants in the media is a challenging work, due to the high amount of anthropogenic compounds released to the environment. Moreover, the different physicochemical properti...

New technological and operational approaches are needed to screen the most toxic contaminants in the environmental and to get insights about their sources, usages and effects on organisms, including human health. The transition from target analysis to non-target analysis through suspect analysis has become a rising field. Recent developments in dat...

The antidepressant amitriptyline is a widely used selective serotonin reuptake inhibitor that is found in the aquatic environment. The present work investigates alterations in the brain and liver metabolome of gilthead bream (Sparus aurata) following exposure at an environmentally relevant concentration (0.2 µg/L) of amitriptyline for 7 days. Analy...

In this work, the full optimisation and validation procedure to analyse a wide set of emerging organic contaminants in biotissues (mussel and fish muscle, liver, gills and brain) and biofluids (fish plasma and bile) is described. The target families include artificial sweeteners, industrial products, hormones, pharmaceutical and personal care produ...

In this study, the spatial and temporal-distribution of 41-multiclass organic compounds were assessed in three estuaries of the Basque Country, from winter 2016 to winter 2017 by grab (active) sampling methods and an extra campaign combining both, grab and passive sampling methods. Wastewater treatment plant (WWTP) effluents were also evaluated to...

The extensive use of the organic UV filter oxybenzone has led to its ubiquitous occurrence in the aquatic environment, causing an ecotoxicological risk to biota. Although some studies reported adverse effects, such as reproductive toxicity, further research needs to be done in order to assess its molecular effects and mechanism of action. Therefore...

The calibration of two passive samplers for the determination of 20 emerging organic compounds in seawater is described in this work: i) a new version of polar organic chemical integrative sampler (POCIS) containing 100 mg of mixed-mode anion exchanger (Strata X-AW) and 100 mg of polymeric HLB (Plexa) sorbent materials and using a highly porous Nyl...

N-ethyl perfluorooctane sulfonamide (EtFOSA) is the active ingredient of Sulfluramid, a pesticide which is used extensively in South America for control of leaf-cutting ants. Despite being a known precursor to perfluorooctane sulfonate (PFOS), the importance of EtFOSA as a source of environmental PFOS remains unclear. In the present work, uptake, l...

The widespread use of pharmaceuticals has caused a growing concern on the presence of pharmaceuticals such as the antibiotic ciprofloxacin (CIPRO) in the aquatic environment, since they may exert adverse effects on non-target organisms, including fish. In order to study the uptake, distribution in different tissues (liver, muscle, brain and gill) a...

A new procedure using polyethersulfone (PES) microextraction followed by liquid chromatography–tandem mass spectrometry (LC–MS/MS) analysis was developed in this work for the simultaneous determination of 41 multiclass priority and emerging organic pollutants including herbicides, hormones, personal care products, and pharmaceuticals, among others,...

Polyfluoroalkyl phosphate esters (PAPs) are high production volume surfactants used in the food contact paper and packaging industry. PAPs may transform to persistent perfluoroalkyl carboxylic acids (PFCAs) under biotic conditions, but little is known about their fate and behavior in aquatic organisms. Here we report for the first time on the uptak...

To achieve a "Good Environmental Status by 2015," as demanded by the water framework directive, monitoring programs are needed to furnish data on target compounds. In this study, a first evaluation of influents and main emissions of 3 local wastewater treatment plants (WWTP) in the Adour estuary (southwest of France) was performed for 23 pollutants...

Ingurumeneko uretan kutsatzaile organiko desberdinak aurkitzen dira nahiz eta kontzentrazio baxuetan izan (ng/L mailan). Araztegien irteera korronteak izan ohi dira konposatu horien iturririk nagusienetako bat, araztegiek erabiltzen dituzten mekanismoak ez baitira gai kutsatzaileen arazketa osoa burutzeko. Horien artean, konposatu disruptore (EDC)...

This work describes the optimization, validation, and application in real samples of accurate and precise analytical methods to determine ten fluoroquinolones (FQs) (norfloxacin, enoxacin, pefloxacin, ofloxacin, levofloxacin, ciprofloxacin, danofloxacin, lomefloxacin, enrofloxacin, and sparfloxacin) in different environmental matrices, such as wate...

Egun, konposatu per- eta polifluoratuek (PFAS-ek) gure eguneroko bizitzan dituzten erabilera anitzak direla eta, ingurunean gero eta nabariagoa da euren presentzia. Ur-ekosistemen egoera aztertzea helburu, organismo itsastarrak kutsaduraren adierazle ezin hobeak dira. Ildo horretan, lan honetan Frantziako, Euskal Herriko, Espainiako eta Portugaleko...

Liquid chromatography coupled to quadrupole time-of-flight mass spectrometry (LC-QToF-MS) was used for the accurate identification (< 10 ppm) of different polyfluoroalkylphosphates (PAPs) and their intermediate and end degradation products in popcorn bags. Up to 46 per- and polyfluoroalkyl substances (PFASs) and precursors were identified. Moreover...

The uptake calibration of three passive samplers, stir-bars, MESCO/stir-bars and polyethersulfone tubes (PESt), was assessed in seawater at different salinities for 17 organic compounds including organochlorine compounds, pesticides, phthalates, musk fragrances and triclosan. The calibration procedure was accomplished by exposing the samplers to a...

Sewage sludge, which acts like a sink for many pollutants, including metals, pathogens and organic pollutants, that are not completely removed in waste water treatment plants (WWTPs), is applied as a nutrient rich organic fertilizer in many agricultural applications. In the present work, carrot and lettuce crops were grown in two different compost...

This study describes a new method for the simultaneous extraction of several endocrine disrupting compounds, including alkylphenols (APs), estrogen, bisphenol-A (BPA) and one phthalate metabolite (mono-2-ethylhexyl ester, MEHP) in fish liver, brain, and muscle. Parameters affecting the extraction (extraction solvent and temperature) and the clean-u...

The uptake calibration of more than 12 non-polar organic contaminants by 3 polymeric materials is shown: bare polydimetilsiloxane (PDMS, stir-bars), polyethersulfone tubes and membranes (PES) and polyoxymethylene membranes (POM), both in their free form and membrane-enclosed sorptive coating (MESCO). The calibration process was carried out exposing...

The uptake of polybrominated diphenyl ethers (PBDEs) by carrot and lettuce was investigated. Degradation of PBDEs in soil in the absence of the plants was discarded. Different carrot (Nantesa and Chantenay) and lettuce (Batavia Golden Spring and Summer Queen) varieties were grown in fortified or contaminated compost-amended soil mixtures under gree...

A simple and fast analytical method for the determination of fourteen perfluorinated compounds (PFCs), including three perfluoroalkylsulfonates (PFSAs), seven perfluorocarboxylic acids (PFCAs), three perfluorophosphonic acids (PFPAs) and perfluorooctanesulfonamide (PFOSA) and ten potential precursors, including four polyfluoroalkyl phosphates (PAPs)...

Abstract The present work studied the uptake of 8:2 perfluoroalkyl phosphate diester (diPAP) by two different crops (lettuce and carrot) and two different amended soils. Firstly, the possible degradation of 8:2 diPAP in the absence of crop was studied and 8:2 monoPAP (monophosphate), 8:2 FTCA (saturated fluorotelomer carboxylate), 8:2 FTUCA (unsatu...

This work describes the optimization, validation, and application in real samples of accurate and precise analytical methods to determine tricyclic antidepressants (TCAs), including amitriptyline, nortriptyline, imipramine, and clomipramine in different environmental matrices, such as water (estuary, seawater, and wastewater treatment plant effluen...

Dispersive liquid-liquid microextraction (DLLME) is a recent microextraction technique that was first developed by Rezaee and co-workers in 2006. It allows the simultaneous extraction and preconcentration of analytes into a micro-volume of extracting solvent based on a ternary solvent system involving an aqueous phase, a nonpolar water immiscible h...

This study describes a new method for the simultaneous extraction and enzymatic hydrolysis of alkylphenols, estrogens, bisphenol-A and phthalate metabolite (mono-2-ethylhexyl ester, MEHP) in fish bile using polyethersulfone (PES) polymer as sorptive material. Parameters affecting the hydrolysis (enzyme amount) and extraction (nature of polymeric ma...

This work describes a new methodology for the simultaneous determination of a large variety of emerging and persistent organic compounds and some of their metabolites in fish bile samples. The target compounds were musk fragrances, alkyl phenols, hormones, pesticides, phthalate esters and bisphenol-A, all of them with a known endocrine disrupting e...

According to the European Water Framework Directive, environmental assessment of organic compounds should be made in whole-water samples, but due to their hydrophobicity and strong attraction to organic content these compounds can be found bound to suspended particle matter or in the dissolved fraction. In this work the extraction of musk compounds...

The development of a simple, cheap and environment friendly analytical method for the simultaneous determination of different perfluoroalkyl substances (PFASs) including seven perfluoroalkyl carboxylic acids, three perfluoroalkane sulfonic acids and perfluorooctanesulfonamide in carrot and amended soil was carried out in the present work. The metho...

The present study is focused on the development of an analytical method based on focused ultrasonic solid-liquid extraction (FUSLE) followed by dispersive solid-phase extraction (dSPE) clean-up and liquid chromatography-triple quadrupole tandem mass spectrometry (LC-MS/MS) optimised for the simultaneous analysis of certain endocrine disrupting comp...

tThe aim of this study was to develop a sensitive and environment-friendly method based on stir-barsorptive extraction (SBSE) followed by thermal desorption–gas chromatography–mass spectrometry(TD–GC–MS) to determine 8 synthetic musks (musk ambrette, musk ketone, celestolide, tonalide, galax-olide, phantolide, traseolide, and cashmeran) in vegetabl...

In the present work, a novel analytical method for the simultaneous determination of ten polybrominated diphenyl ethers (PBDEs), eight methoxylated PBDEs (MeO-PBDEs) and seven hydroxylated PBDEs (OH-PBDEs) in soil, lettuce and carrot samples was developed. The procedure was based on matrix solid-phase dispersion (MSPD) followed by gas chromatograph...

Membrane-assisted solvent extraction (MASE) coupled to liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS) was studied for the determination of a variety of emerging and priority compounds in wastewater. Among the target analytes studied certain hormones (estrone (E1), 17β-estradiol (E2), androsterone (ADT), 17α-ethynyl estradiol (...

Large volume injection (LVI)-in port silylation coupled to gas chromatography-mass spectrometry (GC-MS) for the determination of alkylphenols (APs) in water samples applying four different extraction approaches was evaluated. Among the variables studied for in-port derivatization, vent time, cryo-focusing temperature and the ratio solvent volume/N,...

The aim of this study was to develop a sensitive and environment-friendly method based on stir-bar sorptive extraction (SBSE) followed by thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS) to determine 8 synthetic musks (musk ambrette, musk ketone, celestolide, tonalide, galaxolide, phantolide, traseolide, and cashmeran) in vegetabl...

Focused-ultrasound solid–liquid extraction was developed for the extraction of polybrominated diphenyl ethers in vegetables and amended soil. Firstly, solid-phase extraction clean-up using 2 g and 5 g of Florisil and 2-g silica cartridges were evaluated and elution profile was also optimised. Similar recoveries were obtained for most compounds whil...

In the present work a method was developed for the determination of different perfluorinated compounds (PFCs), including three perfluorinated sulfonic acids (PFSAs), seven perfluorocarboxylic acids (PFCAs), three perfluorophosphonic acids (PFPAs) and perfluorooctanesulfonamide (PFOSA) in fish, vegetables and amended soil samples based on focused ul...

Among the different organic pollutants, persistent organic pollutants and emerging organic contaminants (EOCs) are of particular concern due to their potentially dangerous effects on the ecosystems and on human health. In the framework of the analysis of some of these organic pollutants in water samples, sorptive extraction devices have proven to b...

Endocrine disrupting chemicals (EDCs) interfere with the functioning of the endocrine system, causing reproductive and developmental disturbances in aquatic wildlife. Appearance of intersex gonads and elevated plasma levels of vitellogenin in male fish are well known biomarkers of exposure to xenoestrogenic EDCs. In the present study, intersex cond...