Trabajo presentado en el VII Congreso Argentino de la Sociedad de Toxicologia y Quimica Ambiental, celebrado en San Luis (Argentina), del 16 al 19 de octubre de 2018
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Pharmaceuticals and personal care products (PPCPs) are abundantly used by people, and some of them are excreted unaltered or as metabolites through urine, with the sewage being the most important source to their release to the... more
Pharmaceuticals and personal care products (PPCPs) are abundantly used by people, and some of them are excreted unaltered or as metabolites through urine, with the sewage being the most important source to their release to the environment. These compounds are in almost all types of water (wastewater, surface water, groundwater, etc.) at concentrations ranging from ng/L to µg/L. The isolation and concentration of the PPCPs from water achieves the appropriate sensitivity. This step is mostly based on solid-phase extraction (SPE) but also includes other approaches (dispersive liquid-liquid microextraction (DLLME), buckypaper, SPE using multicartridges, etc.). In this review article, we aim to discuss the procedures employed to extract PPCPs from any type of water sample prior to their determination via an instrumental analytical technique. Furthermore, we put forward not only the merits of the different methods available but also a number of inconsistencies, divergences, weaknesses and...
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Abstract Water bodies cover approximately 70 % of the earth´s surface, making them ecosystems with a high environmental value and the habitat for numerous species of flora and fauna. Emerging pollutants (EPs) are ubiquitous anthropogenic... more
Abstract Water bodies cover approximately 70 % of the earth´s surface, making them ecosystems with a high environmental value and the habitat for numerous species of flora and fauna. Emerging pollutants (EPs) are ubiquitous anthropogenic compounds of environmental concern that can be found at different concentration levels in matrices such as sediment, water and aquatic biota. In addition, EPs can be bioaccumulated and biomagnified, inducing adverse effects on biota, and posing a risk to humans when contaminated biota is consumed. Unlike abiotic matrices, the occurrence of EPs in aquatic biota has not been widely studied. This is probably because their complexity, due to the presence of lipids, proteins and other organic compounds, makes the extraction and analysis of EPs difficult. This review gathers the most relevant analytical methods published between 2014 and 2019, comparing them and evaluating their strengths and weaknesses. It is intended to provide a better understanding of the development of new and improved methods, and to be a reference for researchers who are looking for the best methodology for their studies.
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Pest control in agriculture is mainly based on the application of insecticides, which may impact nontarget beneficial organisms leading to undesirable ecological effects. Neonicotinoids are among the most widely used insecticides.... more
Pest control in agriculture is mainly based on the application of insecticides, which may impact nontarget beneficial organisms leading to undesirable ecological effects. Neonicotinoids are among the most widely used insecticides. However, they have important negative side effects, especially for pollinators and other beneficial insects feeding on nectar. Here, we identify a more accessible exposure route: Neonicotinoids reach and kill beneficial insects that feed on the most abundant carbohydrate source for insects in agroecosystems, honeydew. Honeydew is the excretion product of phloem-feeding hemipteran insects such as aphids, mealybugs, whiteflies, and psyllids. We allowed parasitic wasps and pollinating hoverflies to feed on honeydew from hemipterans feeding on trees treated with thiamethoxam or imidacloprid, the most commonly used neonicotinoids. LC-MS/MS analyses demonstrated that both neonicotinoids were present in honeydew. Honeydew with thiamethoxam was highly toxic to bot...
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The current literature about pharmaceutical and personal care compounds (PPCPs) focuses on identifying their concentration and toxicological risk both in surface water and in wastewater. However, the influence of urban areas (population... more
The current literature about pharmaceutical and personal care compounds (PPCPs) focuses on identifying their concentration and toxicological risk both in surface water and in wastewater. However, the influence of urban areas (population ageing, income level, hospitals and others) has not yet been analysed. Knowing how a population (and its facilities) affects PPCPs' presence in wastewater is important to identify the conditions that are responsible for their presence. In this work, the influence of water consumption, population ageing, income level, hospitals and nursing homes on the anti-inflammatory concentration have been analysed. To fill the gap between the quantitative data on PPCPs' concentration and the qualitative reasoning of the influence of urban areas on the anti-inflammatory concentration, the use of fuzzy-set qualitative comparative analysis (fsQCA) is proposed. The fsQCA results are presented as recipes that show the different causal combinations of conditions that explain the presence of anti-inflammatories in wastewater. Using fsQCA for urban wastewater management with the aim of explaining the presence of anti-inflammatories in wastewater treatment plants (WWTPs) is a novelty in the literature. The results obtained here show the influence of water consumption (WATCON), hospitals (HOSP) and population ageing (POPAG) as the main conditions for the anti-inflammatory concentration in Valèncian wastewater. Specifically, these conditions are present in all the recipes obtained with consistency of 99%. Through the results obtained, it would be possible to identify that HOSP are the main facilities that discharge anti-inflammatories into urban wastewater. Hence, the necessity of preventive measures to avoid the anti-inflammatory discharge into water bodies has been showed. Furthermore, under a methodological point of view, this work highlights the eligibility of fsQCA as a wastewater cycle management tool.
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A solid-liquid extraction method in combination with high-performance liquid chromatography and tandem mass spectrometry was developed and optimized for extraction and analysis of organophosphorus flame retardants in soil and fish.... more
A solid-liquid extraction method in combination with high-performance liquid chromatography and tandem mass spectrometry was developed and optimized for extraction and analysis of organophosphorus flame retardants in soil and fish. Methanol was chosen as the optimum extraction solvent, not only in terms of extraction efficiency, but also for its broader analyte coverage. The subsequent clean-up by solid-phase extraction is required to eliminate matrix coextractives and reduce matrix effects. Recoveries of the optimized method were 50-121% for soil and 47-123% for biota, both with high precision (RSDs <12% in soil and <23% in biota). The method limits of detection ranged from 0.06 to 0.20 ng/g dry weight and between 0.02 and 0.30 ng/g wet weight for soil and biota samples, respectively. However, samples with a high lipid content produce several problems as solid-phase extraction cartridge clogging that increase variability and analysis time. The method was successfully applied ...
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The presence of pharmaceutical and personal care products and drugs of abuse (PPCPs) in wastewater treatment plants (WWTPs) indicates discharge of the effluent may not be suitable for the ecological balance of water ecosystems, such as... more
The presence of pharmaceutical and personal care products and drugs of abuse (PPCPs) in wastewater treatment plants (WWTPs) indicates discharge of the effluent may not be suitable for the ecological balance of water ecosystems, such as wetlands. These PPCPs degrade water quality, considered as an ecosystem service (ES), provoking serious environmental impacts. Assessing the monetary value of PPCPs can be used as a proxy for environmental status of the ES of water quality (ESWQ). Considering PPCPs as non-desirable outputs of WWTPs, the shadow prices methodology has been implemented using directional distance function to measure the environmental avoided cost of removing salicylic acid (SA), methylparaben (MP), and THCOOH from WWTPs effluents discharged to Albufera Natural Park (Spain). The SA shows the highest shadow price (138.16 €/μg), followed by THCOOH (48.15 €/μg), and MP (30.66 €/μg). These values are interpreted as the environmental cost that would be avoided if SA, MP, and TH...
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The occurrence of pesticide residues in fruits was determined by a target method for 62 analytes and a wide scope screening method against a database of 500 pesticides. Limits of quantification (LOQs) were from 0.5 to 6.3 μg kg(-1) for... more
The occurrence of pesticide residues in fruits was determined by a target method for 62 analytes and a wide scope screening method against a database of 500 pesticides. Limits of quantification (LOQs) were from 0.5 to 6.3 μg kg(-1) for the target method and from 0.5 to 119 μg kg(-1) for the non-target. Thirty samples: dates, apples, oranges, tangerines, lemons and grapefruits were selected because their high consumption, except lemons and grapefruits that were to cover all citrus fruits. Using the target method, 15 compounds (mostly insecticides and fungicides) out of 62 pesticides (organophosphorus, carbamates, pyrethroids, chloroacetanilides, triazines, triazoles, imidazoles, etc.) were detected. Residues were in 100% of the samples, 80% contained at or below maximum residue limits (MRLs), and 20% above. Non-target method identified several additional pesticides (cypronil, fludioxonil, boscalid and pyraclostrobin in apples). The highest acute risk were for achrinathrin, chlorpyrif...
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An analytical method using a quick, easy, cheap, effective, rugged and safe (QuEChERS) procedure for multi-residue determination of 52 pesticides in coffee leaf extractshas been developed and validated according to SANTE/11945/2015... more
An analytical method using a quick, easy, cheap, effective, rugged and safe (QuEChERS) procedure for multi-residue determination of 52 pesticides in coffee leaf extractshas been developed and validated according to SANTE/11945/2015 guidelines. Different sorbent combinations for dispersive solid phase extraction (d-SPE) clean-up as well as dispersive liquid-liquid microextraction (DLLME) were tested. The relative standard deviations (RSDs) for the recovery of 87-94% of pesticides added to coffee leaf extracts,was ≤20% for samples spiked at concentrations up to 50ng*g depending on the clean-up procedures. However, samples spiked with a 100ng*g pesticide mixture gave RSDs&gt;20% for most pesticides when d-SPE was carried out adding Supelclean ENVI-Carb 120/400. To explain this fact,the secondary metabolic profile was analyzed in all the extraction and clean-up procedures. Only in the clean-up procedure with the addition of Supel QuE Z-Sep+, does caffeine show a constant adsorption between blank and spiked samples. In other clean-up procedures, the amount of caffeine was higher in those samples spiked with pesticides. This indicates competition between caffeine and pesticides for adsorption to the sorbent. Addition of Supel QuE Z-Sep+ to the procedure revealed only a 32% matrix effect, whereas using PSA+ C18 the matrix effect was close to 97%. The process efficiency is up to 54% with the addition of Supel QuE Z-Sep+ and just up to 7% for the other clean-up procedures. The method was successfully tested in coffee leaves from different types of cultivars. Pesticides were not detected in organic coffee leaf extracts, but thiametoxan was clearly detected in 50% of coffee leaf extracts harvested from coffee trees grown under traditional conditions as determined by UHPLC-TOFMSLC/QqTOF-MS/MS.
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A combined methodology to identify and quantify farming chemicals in the entire Júcar River basin has been developed. The procedure consisted of the application of environmental forensic criteria associating laboratory analytical samples,... more
A combined methodology to identify and quantify farming chemicals in the entire Júcar River basin has been developed. The procedure consisted of the application of environmental forensic criteria associating laboratory analytical samples, cartographic analysis using Geographical Information Systems (GIS) and synthetic statistical analysis. Sampling involved the collection of 15 samples in surface waters distributed alongside the Júcar River and its two main tributaries (Cabriel and Magro Rivers). The analytical procedure involves generic sample extraction and selective determination of up to 50 target pesticides by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). Geographical analysis was performed by mixing both sampling points with analytical results and land use-cover layers for the year 2011. PCA and descriptive statistical analysis was further performed combining land use/cover information and pesticides results to determine correlation between dominant agricultural practices (irrigation and rain fed farming) and location of sampling points. Out of 50 pesticides, 20 were identified and 18 presented concentrations higher than the limits of quantification in surface waters, with a large dispersion in concentrations: from 0.05ng/L (terbuthylazine-2 hydroxy) to 222.45ng/L (imazalil). Statistical analyses reveals that there is a correlation between the percentage of land devoted to irrigation farming, whereas correlations are weaker when analysing the relationship of pesticides in rain fed dominated areas.
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HIGHLIGHTSMethod characterization for 47 organic contaminants in water, soil, sediment and fish.SLE with McIlvain‐EDTA (pH = 4.5) and methanol to extract the solid matrices.SPE to clean‐up the extract used also to extract different types... more
HIGHLIGHTSMethod characterization for 47 organic contaminants in water, soil, sediment and fish.SLE with McIlvain‐EDTA (pH = 4.5) and methanol to extract the solid matrices.SPE to clean‐up the extract used also to extract different types of water samples.Contaminants widely distributed particularly in water but also in other matrices.Degree of contamination water >> sediment > soil > biota. ABSTRACT A sensitive and reliable method based on solid‐liquid extraction (SLE) using McIlvaine‐Na2EDTA buffer (pH = 4.5)‐methanol and solid‐phase extraction (SPE) clean up prior to ultra‐high‐performance liquid chromatography coupled to tandem mass spectrometry (UHPLC–MS/MS) was applied to determine 47 organic contaminants in fish, soil and sediments. The SPE procedure to clean‐up the extracts was also used as extraction method to determine these compounds in water. Recoveries ranged from 38 to 104% for all matrices with RSDs < 30%. Limits of Quantification for the target compounds were in the range of 10–50 ng/g for soil, 2–40 ng/g for sediment, 5–30 ng/g for fish and 0.3–26 ng/L for water. Furthermore, the proposed method was compared to QuEChERS (widely used for environmental matrices) that involves extraction with buffered acetonitrile (pH 5.5) and dispersive SPE clean‐up. The results obtained (recoveries>50% for 36 compounds in front of 9, matrix effect < 20% for 31 compounds against 21, and LOQs <25 ng g−1 for 38 compounds against 22) indicates that the proposed method is more efficient than QuEChERS, The method was applied to monitoring these compounds along the Turia River. In river waters, Paracetamol (175 ng L−1), ibuprofen (153 ng L−1) and bisphenol A (41 ng L−1) were the compounds most frequently detected while in sediments were vildagliptin (7 ng g−1) and metoprolol (31 ng g−1) and in fish, bisphenol A (33 ng g−1) or sulfamethoxazole (13 ng g−1).
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A new selective and sensitive liquid chromatography triple quadrupole mass spectrometry method was developed for simultaneous analysis of natural pyrethrins and synthetic pyrethroids residues in baby food. In this study, two sample... more
A new selective and sensitive liquid chromatography triple quadrupole mass spectrometry method was developed for simultaneous analysis of natural pyrethrins and synthetic pyrethroids residues in baby food. In this study, two sample preparation methods based on ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) and salting-out assisted liquid-liquid extraction (SALLE) were optimized, and then, compared regarding the performance criteria. Appropriate linearity in solvent and matrix-based calibrations, and suitable recoveries (75-120%) and precision (RSD values≤16%) were achieved for selected analytes by any of the sample preparation procedures. Both methods provided the analytical selectivity required for the monitoring of the insecticides in fruit-, cereal- and milk-based baby foods. SALLE, recognized by cost-effectiveness, and simple and fast execution, provided a lower enrichment factor, consequently, higher limits of quantification (LOQs) were obtained. Some o...
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Monitoring of pesticides and veterinary drug residues is required to enforce legislation and guarantee food safety. Liquid chromatography-mass spectrometry (LC-MS) is the prevailing technique for assessing both types of residues because... more
Monitoring of pesticides and veterinary drug residues is required to enforce legislation and guarantee food safety. Liquid chromatography-mass spectrometry (LC-MS) is the prevailing technique for assessing both types of residues because LC offers a versatile and universal separation mechanism suitable for non-gas chromatography (GC) amenable and the majority of GC-amenable compounds. This characteristic becomes more relevant when LC is coupled to MS because the high sensitivity and specificity of the detector allows to apply generic sample preparation procedures, which simultaneously extract a wide variety of residues with different physico-chemical properties. Determination of metabolites and degradation products, non-target suspected screening of an increasing number of residues, and even unknowns identification are also becoming inherent LC-MS advantages thanks to the latest advances. For routine analysis and, in particular, for official surveillance purposes in food control, analytical methods properly validated following strict guidelines are needed. After a brief introduction and an outline of the legislation applicable around the world, aspects such as improvement of specificity of high-throughput methods, resolution and mass accuracy of identification strategies and quantitative accuracy are critically reviewed in this article. In them, extraction, separation and determination are emphasized. The main objective is to offer an assessment of the state of the art and identify research needs and future trends in determining pesticide and veterinary drug residues in food by LC-MS.
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The determination of the real toxicity of sediments in aquatic ecosystems is challenging and necessary for an appropriate risk assessment. Different approaches have been developed and applied over the last several decades. Currently, the... more
The determination of the real toxicity of sediments in aquatic ecosystems is challenging and necessary for an appropriate risk assessment. Different approaches have been developed and applied over the last several decades. Currently, the joint implementation of chemical, ecological and toxicological tools is recommended for an appropriate and successful toxicity risk assessment. We chose the combination of the toxic unit approach with acute pore water tests (Vibrio fischeri, Pseudokirchneriella subcapitata and Daphnia magna) and whole-sediment exposure tests (V. fischeri, Chironomus riparius), together with invertebrate community composition (multivariate analyses) to detect short and long-term responses of the organisms in four rivers of the Iberian Peninsula. High toxicity was detected in three sites (the downstream sites of the Llobregat and the Júcar, and the most upstream site of the Ebro). We identified organophosphate insecticides and metals as the main variables responsible ...
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Coastal wetlands are areas that suffer from great pressure. Much of it is due to the rapid development of the surrounding artificial landscapes, where socio-economic factors lead to alterations in the nearby environment, affecting the... more
Coastal wetlands are areas that suffer from great pressure. Much of it is due to the rapid development of the surrounding artificial landscapes, where socio-economic factors lead to alterations in the nearby environment, affecting the quality of natural and agricultural systems. This work analyses interconnections among landscapes under the hypothesis that urban-artificial impacts could be detected on soils and waters of an agro-ecological protected area, L'Albufera de Valencia Natural Park, located in the vicinity of the City of Valencia, Spain. The methodological framework developed addresses two types of anthropogenic pressure: (1) direct, due to artificialisation of soil covers that cause soil sealing, and (2) indirect, which are related to water flows coming from urban populations through sewage and irrigation systems and which, ultimately, will be identified by the presence of emerging pharmaceutical contaminants in waters of the protected area. For soil sealing, a methodo...
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Acetonitrile extraction followed by primary-secondary amine dispersive SPE cleanup QuEChERS (quick, easy, cheap, effective, rugged, and safe), was compared to pressurized liquid extraction (PLE) using water at 70 degrees C for 10 min at... more
Acetonitrile extraction followed by primary-secondary amine dispersive SPE cleanup QuEChERS (quick, easy, cheap, effective, rugged, and safe), was compared to pressurized liquid extraction (PLE) using water at 70 degrees C for 10 min at 1500 psi for the determination of 16 veterinary drugs in bovine muscle tissues by LC/MS/MS. PLE was significantly more effective for the extraction of veterinary drugs (ranging from 69 to 103% with RSD < or = 18%) than QuEChERS (ranging from 19 to 89% with RSD < or = 19%). Linearity of the calibration curves was obtained over the range considered from 10 microg/kg or LOQ to 1000, microg/kg) with r2 > or = 0.99 for all the analytes by both methods. Although an internal standard was used, matrix effects were corrected using matrix- matched standards. LODs were from 5 to 30 microg/kg for PLE and from 10 to 100 microg/kg for QuEChERS. To establish and assess the most efficient conditions for each extraction method, statistical parametric and non...
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Perfluorinated compounds are industrial chemicals widely used for more than 60 years. However, during the last decade, due to their high resistance to degradation, bioaccumulation attached to proteins, biomagnification to the food chain... more
Perfluorinated compounds are industrial chemicals widely used for more than 60 years. However, during the last decade, due to their high resistance to degradation, bioaccumulation attached to proteins, biomagnification to the food chain and their relation to toxicological effects of these compounds have gained scientific and regulatory attention.
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... Capillary Gas Chromatography M. Jesus Redondo, Yolanda Pico, Juan Server-Carri6*, Jorge Maiies, and Guillermina Font Laboratory of Food Chemistry and Toxicology, Faculty of Pharmacy, University of Valencia, 4601 0 Valencia, Spain ...
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ABSTRACT The application of SPE technology to the isolation of pesticides and related compounds from food and soils has grown enormously in the last decade. Much of this growth has been due to the relative ease of sample handling and the... more
ABSTRACT The application of SPE technology to the isolation of pesticides and related compounds from food and soils has grown enormously in the last decade. Much of this growth has been due to the relative ease of sample handling and the wide range of solid supports currently available for a variety of applications. The aim of this review is to present the methods for solid phase extraction (SPE) of pesticide residues from soils and foods. There are three main areas according to the type of approach used to handle the sample: solid phase extraction, solid phase clean-up (SPC), and matrix solid phase dispersion (MSPD). This review covers milk products, fatty foods, fruits, vegetables, and soils. Solid phase materials are discussed in each case in terms of reversed bonded-phase silica sorbents (C18, C8, C2, etc.) and polar sorbents (alumina, Florisil, and silica).
ABSTRACT The Mediterranean wetlands are unique in biological diversity and provide multiple benefits, constituting a great water reserve for the planet and producing biomass and nutrients for the trophic chain. However, the increasing... more
ABSTRACT The Mediterranean wetlands are unique in biological diversity and provide multiple benefits, constituting a great water reserve for the planet and producing biomass and nutrients for the trophic chain. However, the increasing human impact and socio-economic development in recent decades have caused important losses in these ecosystems. This work was carried out in the Natural Park of L’Albufera (Valencia, Spain), which includes a coastal lagoon, marshlands, dunes and pinewoods, surrounded by rice fields and orchard in its non-urbanized part. Despite this great ecological value, it suffers impacts derived from the high human and industrial occupation and the hydrological contributions of the connected irrigation systems. The study focused on the development of a combined methodology, based on environmental forensics principles, with the aim of identifying the presence, flow paths and spatial distribution of illicit drugs entering the Natural Park. It is organized around two major procedures: analysis of 16 water samples and application of Geographical Information Systems (GIS) integrating different sources and data formats, as analysis of 14 drugs of abuse by Liquid Chromatography-Mass Spectrometry techniques, and social and environmental data in either GIS layers or tabular digital formats. Results show that, at present, most analyzed drugs have been identified in all sample points. Besides the population distribution pattern, the traditional irrigation system connected to sewage treatment plant (STP) locations is the way by which illicit substances are introduced into the Natural Park waters.
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Pressurized liquid extraction (PLE) and Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) extraction methods were optimized for the simultaneous determination of 50 pesticides in sediment, soils and sewage sludge. For QuEChERS... more
Pressurized liquid extraction (PLE) and Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) extraction methods were optimized for the simultaneous determination of 50 pesticides in sediment, soils and sewage sludge. For QuEChERS development, several buffers and dispersive solid-phase extraction clean-up (dSPE) sorbents were tested. In the PLE method, several parameters affecting the extraction efficiency, such as organic solvent, amount of sample, cell size, temperature, pressure, static time, number of cycles and % of flush, as well as sorbent used for the on-line clean up, were also evaluated. PLE and QuEChERS were assessed and compared in obtained recoveries (33-89% versus 25-120%), number of pesticides for which recoveries are in the range of 80-100% (up to 13 versus up to 35) and cost of the approach. QuEChERS procedure was faster, cheaper and easier to perform. Recoveries were around 80% (at 50ngg(-1) d.w.) and the matrix effect was less than -20% using matrix-matched standard calibration curve for most of the analytes. The limits of quantification were between 0.1 and 10ngg(-1) (d.w.) except for alachlor and acetochlor. Repeatability and reproducibility were lower than 28% (%RSD, n=5). Soil, sediment and sludge samples, taken from the Túria River Basin, were analyzed by QuEChERS to determine pesticides. Chlorpyrifos (up to 65.3ngg(-1) d.w.) was the most frequent and at higher concentrations. Thiabendazole, imazalil, diazinon, pyriproxyfen, hexythiazox, carbofuran, isoproturon, terbuthylazine and terbumeton were also found in some samples.
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Nanotechnology has emerged as one of the most innovative technologies and has the potential to improve food quality and safety. However, there are a few studies demonstrating that nanomaterials (NMs) are not inherently benign.This review... more
Nanotechnology has emerged as one of the most innovative technologies and has the potential to improve food quality and safety. However, there are a few studies demonstrating that nanomaterials (NMs) are not inherently benign.This review highlights some current applications of NMs in food, food additives and food-contact materials, and reviews analytical approaches suitable to address food-safety issues related to nanotechnology.We
Research Interests: Analytical Chemistry, Food Safety, Electron Microscopy, Light Scattering, Chromatography, and 15 moreMass Spectrometry, Imaging, Nanoparticle, Raman Spectroscopy, Nanotechnology, Sample Preparation, Food Analysis, Food Quality, Food Packaging, Application, Food Additives, Cover, Food Additive, Nanomaterial, and Raman Scattering
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Research Interests: Chemistry, Mass Spectrometry, Wastewater Treatment, Medicine, Multidisciplinary, and 15 moreForest soil nutrition, Soil contamination, Sewage sludge, Solid Phase Extraction, Waste Water Treatment Plant, Nonylphenol, High Pressure Liquid Chromatography, Liquid Chromatography / Electrospray Ionization Mass Spectrometry, Phenols, Liquid Chromatography, Sewage, Fertilizers, Ethers, Soil Pollutants, and Production Rate
Water has been identified as one of the main routes of human exposure to perfluoroalkyl substances (PFASs). This work assessed the presence of 21 PFASs along the whole water cycle using a new fast and cost effective analytical method... more
Water has been identified as one of the main routes of human exposure to perfluoroalkyl substances (PFASs). This work assessed the presence of 21 PFASs along the whole water cycle using a new fast and cost effective analytical method based on an online sample enrichment followed by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). The method was validated for different types of matrices (ultrapure water, tap water and treated wastewater). The quality parameters for the 21 selected compounds presented good limits of detection (LOD) and quantification (LOQ) ranging, in general, from 0.83-10 ng/L to 2.8-50 ng/L, respectively. The method was applied to assess the occurrence of PFASs in 148 water samples of different steps along the whole water cycle, including: mineral bottled water, tap water, river water and treated effluent wastewater, from Germany to Spain. In addition, in order to prove the good performance of the online analytical method, the analysis of PFASs was carried out in parallel using a method based on offline anionic solid phase extraction (SPE) followed by LC-MS/MS. Consistent results were obtained using both approaches. The more frequently found compounds were perfluoroalkyl acids, such as the perfluorobutanoic acid which was in the 54% of the tap water samples investigated with concentrations in the range between 2.4 and 27 ng/L, the perfluoroheptanoic acid (0.23-53 ng/L) and perfluorooctanoic acid (0.16-35 ng/L), and the sulphonate perfluorooctanesulfonate (0.04-258 ng/L) which was the second more frequent compound and also the compound found in with the higher concentration. It should be remarked that the 88% of the samples analyzed presented at least one of the compounds at quantifiable concentrations. In addition, PFASs including short chain compounds were proved to be prevalent in drinking water, and the 50% of the drinking water samples showed quantifiable concentrations of PFASs. It should be said that the great majority of the samples may not pose an immediate health risk to consumers, and just 6 of the drinking water samples presented concentrations of PFOS exceeding the Provisional Health Advisory (PHA) level established by the Office of Water from the USEPA for PFOS, which was set in 200 ng/L.
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Research Interests: Analytical Chemistry, Mass Spectrometry, Pesticide Residues, Time-of-flight mass spectrometry, Food Analysis, and 14 moreInsecticides, Pesticide, Pesticides, Tandem Mass Spectrometry, Chemical Analysis, Contamination, Herbicides, High Pressure Liquid Chromatography, Liquid Chromatography, Pollutant, Food Contamination, Environmental Pollutants, Residue, and Environment
Research Interests: Chemistry, Analytical Chemistry, Food Safety, Mass Spectrometry, Pesticide Residues, and 14 moreMedicine, Time-of-flight mass spectrometry, Food Analysis, Pesticide, Pesticides, Tandem Mass Spectrometry, High Pressure Liquid Chromatography, Liquid Chromatography / Electrospray Ionization Mass Spectrometry, Liquid Chromatography, Food Contamination, Residue, Sensitivity and Specificity, LC MS, and HPLC Chromatography
This review addresses recent advances in the analysis of organic contaminants, such as antibiotics, pesticides, biological toxins, and food-borne pathogens, in foods by capillary electrophoresis (CE). Special attention is paid to those... more
This review addresses recent advances in the analysis of organic contaminants, such as antibiotics, pesticides, biological toxins, and food-borne pathogens, in foods by capillary electrophoresis (CE). Special attention is paid to those aspects that increase sensitivity and/or selectivity, such as sample extraction and concentration, on-line preconcentration techniques (stacking), affinity capillaries or/and specific detectors (laser induced fluorescence (LIF), mass spectrometry (MS)). The various CE modes used to separate the compounds and the quantification strategies are also examined. As a result, this work presents an updated overview on the principal applications of CE, together with a discussion of their main advantages and drawbacks, and an outline of future trends in the analysis of organic contaminants in food.
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Removal of contaminants in the sewage treatment plants (STPs) can be incomplete causing their release to the environment. In this paper, the results of an extensive survey on more than 40 pesticides carried out in 2010 and 2011 in 16 STPs... more
Removal of contaminants in the sewage treatment plants (STPs) can be incomplete causing their release to the environment. In this paper, the results of an extensive survey on more than 40 pesticides carried out in 2010 and 2011 in 16 STPs of Ebro, Guadalquivir, Jucar and Llobregat Rivers (Spain) are presented. In 2010, of 43 analytes screened, 29 were detected in influent and 28 in effluent samples, meanwhile in 2011, of 50 analytes, 33 and 34 were detected, respectively. Pesticides were in the range of 0.33 ng L(-1) (terbumeton, 2011)-2526.05 ng L(-1) (diuron, 2010) for influent and 0.25 ng L(-1) (terbumeton, 2011)-2821.12 ng L(-1) (carbendazim, 2011) for effluent. Regarding the sludge samples, 11 pesticides were detected in 2010 and 24 in 2011 at concentrations up to 25667.34 ng g(-1) dry weight (dw). Removal efficiencies showed that, in 2010, the elimination ranged from -810% (chlorfenvinphos) to 93% (dimethoate), and in 2011, from -4575% (diazinon) to 97% (chlorfenvinphos). All these data confirm that most of the pesticides are only partially eliminated during the secondary and even tertiary treatments, commonly used in STPs, suggesting that they can be a focal point of contamination to the rivers.
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Research Interests: Engineering, Chemistry, Food Safety, Mass Spectrometry, Pesticide Residues, and 15 moreMedicine, Electrospray, Pesticide, Calibration, Fruit, Chemical Analysis, Contamination, High Performance Liquid Chromatography, CHEMICAL SCIENCES, Liquid Chromatography, LC MS, Dynamic Range, Fungicide, measurement accuracy, and limit of detection
Research Interests: Engineering, Chemistry, Mass Spectrometry, Pesticide Residues, Medicine, and 15 moreFood Analysis, Electrospray, Pesticide, Pesticides, Legislation, Chemical Analysis, Contamination, CHEMICAL SCIENCES, Beverages, Liquid Chromatography, LC MS, Carbamates, Fruit Juice, Electrospray Ionization, and HPLC Chromatography
Research Interests: Engineering, Chemistry, Technology, Mass Spectrometry, Pesticide Residues, and 15 moreMedicine, Linear models, Insecticides, Honey, Solid Phase Extraction, Pesticides, Solid Phase Microextraction, High Pressure Liquid Chromatography, CHEMICAL SCIENCES, Liquid Chromatography, Reproducibility of Results, Extraction Method, Sensitivity and Specificity, SPE, and Relative Standard Deviation
Research Interests: Engineering, Technology, Water, Everyday Life, Sewage sludge, and 15 moreWaste water treatment, Solvent Extraction, Solid Phase Extraction, Methanol, Tandem Mass Spectrometry, Waste Water Treatment Plant, CHEMICAL SCIENCES, Liquid Chromatography, Sewage, Reproducibility of Results, Environmental Pollutants, Sensitivity and Specificity, Physicochemical Properties, Mass Spectrometer, and limit of detection
Research Interests: Engineering, Chemistry, Technology, Mass Spectrometry, Pesticide Residues, and 12 moreMedicine, Food Analysis, Pesticides, Citrus, High Pressure Liquid Chromatography, CHEMICAL SCIENCES, Structure Elucidation, Analytical Method, Liquid Chromatography, Reproducibility of Results, Sensitivity and Specificity, and Carbamates
Research Interests: Engineering, Chemistry, High Pressure, Mass Spectrometry, Pesticide Residues, and 15 moreMedicine, Quantitative analysis, Identification, Pesticide, Pesticides, Fruit, Chemical Analysis, Contamination, High Pressure Liquid Chromatography, Qualitative Analysis, CHEMICAL SCIENCES, Acaricide, Liquid Chromatography, Quantitative Analysis, and Relative Standard Deviation
Liquid chromatography-triple quadrupole/mass spectrometry (LC-TQ/MS) and liquid chromatography-quadrupole ion trap/mass spectrometry (LC-QIT/MS) for determining bupirimate, hexaflumuron, tebufenpyrad, buprofezin, pyriproxyfen, and... more
Liquid chromatography-triple quadrupole/mass spectrometry (LC-TQ/MS) and liquid chromatography-quadrupole ion trap/mass spectrometry (LC-QIT/MS) for determining bupirimate, hexaflumuron, tebufenpyrad, buprofezin, pyriproxyfen, and fluvalinate in fruits have been compared. The differences in the mass spectra obtained by triple and ion trap quadrupoles are discussed, showing how both of them provide interesting features. The evaluation of the two instruments was carried out by ethyl acetate extraction of oranges spiked with the studied pesticides at LOQ and 10 times the LOQ. Results obtained by LC-TQ/MS correlated well with those obtained by LC-QIT/MS. Recoveries were 70-94% by LC-TQ/MS and 72-92% by LC-QIT/MS with the R.S.D. from five replicate analysis 4-14% and 8-18%, respectively. Matrix effects were tested for both techniques by standard addition to blank extracts. Although the matrix effects are not originated in mass analyzer but in the LC/MS interface, they were, generally, more marked by LC-QIT-MS than by LC-TQ/MS. The limits of quantification (LOQs) were 0.005-0.2 mg kg(-1) by both equipments--appropriate values for determining these pesticides in orange from the regulatory point of view. The results indicate that the TQ provides higher precision, better linearity, it is more robust, and when the purpose of the analysis is quantitative determination, preferable over the QIT. However, the application of both mass spectrometers to analyze orange samples conventionally treated showed that any can be used for qualitative and quantitative purposes.