0000000000175036
AUTHOR
Ana Masiá
showing 18 related works from this author
Distribution and fate of perfluoroalkyl substances in Mediterranean Spanish sewage treatment plants.
2014
The concentrations of 21 perfluoroalkyl substances (PFASs: C4-C14, C16, C18 carboxylates, C4, C6-C8 and C10 sulfonates and C8 sulfonamide) were determined in influent, effluent and sludge from 16 different sewage treatment plants (STPs) located in the Ebro (6), Guadalquivir (5), Jucar (2) and Llobregat (3) Rivers, in two consecutive years (2010 and 2011). The analytes were extracted by solid phase extraction (SPE) and determined by Liquid Chromatography triple Quadrupole Mass Spectrometer (LC-QqQ-MS). All samples, except two sludges from Guadalquivir River STPs, were contaminated with at least one PFAS. Perfluorobutanoate (PFBA), perfluoropentanoate (PFPeA) and perfluorooctane sulfonate (L-…
Procedures for Antibiotic Residues in Bovine Muscle Tissues
2011
Abstract 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°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 ≤ 18%) than QuEChERS (ranging from 19 to 89% with RSD ≤ 19%). Linearity of the calibration curves was obtained over the range considered (from 10 μg/kg or LOQ to 1000, μg/kg) with r2 ≥ 0.99 for all the analytes by both methods. Although an internal standard w…
Pesticide occurrence in the waters of Júcar River, Spain from different farming landscapes.
2017
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). Geogra…
Combined use of liquid chromatography triple quadrupole mass spectrometry and liquid chromatography quadrupole time-of-flight mass spectrometry in sy…
2012
As a suitable way for routine screening of pesticides and control of other organic contaminants in water, the combination of liquid chromatography triple quadrupole tandem mass spectrometry (LC-QqQ-MS/MS) and liquid chromatography-hybrid quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) has been applied to the analysis of 63 surface and waste water samples after conventional solid-phase extraction (SPE). The extracts were screened for 43 pesticides or degradation products by LC-QqQ-MS/MS achieving limits of detection (LOD) ranged from 0.04 to 2 ng L(-1). Of the 43 selected pesticides, 33 were detected in water samples. The ESI-QTOF MS instrument was run using two simultaneous acquisi…
Determination of pesticides and veterinary drug residues in food by liquid chromatography-mass spectrometry: A review
2015
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 …
Patterns of presence and concentration of pesticides in fish and waters of the Júcar River (Eastern Spain).
2013
The Jucar River, in a typical Mediterranean Basin, is expected to suffer a decline in water quality and quantity as a consequence of the climate change. This study is focused on the presence and distribution of pesticides in water and fish, using the first extensive optimization and application of the QuEChERS method to determine pesticides in freshwater fish. Majority pesticides in water - in terms of presence and concentration - were dichlofenthion, chlorfenvinphos, imazalil, pyriproxyfen and prochloraz (associated with a frequent use in farming activities), as well as buprofezin, chlorpyriphos and hexythiazox. In fish, the main compounds were azinphos-ethyl, chlorpyriphos, diazinon, dime…
Screening of currently used pesticides in water, sediments and biota of the Guadalquivir River Basin (Spain)
2013
The occurrence of 50 currently used pesticides and their transformation products in surface and waste waters, sediment and fish in the Guadalquivir River Basin was determined in 2010 and 2011. After selective sample extraction, pesticides were identified and quantified by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). The contamination profile in water and sediments is marked by the presence of organophosphorus and triazines. Transformation products were even at higher concentrations than parent pesticides. A wider range of pesticides was present in water than in sediments but none of them were detected in fish. The mean concentrations ranged from 0.2 to 13.0 ng/L in …
Assessment of two extraction methods to determine pesticides in soils, sediments and sludges. Application to the Túria River Basin.
2014
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%)…
Occurrence and removal efficiency of pesticides in sewage treatment plants of four Mediterranean River Basins.
2013
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 sam…
Pesticide monitoring in the basin of Llobregat River (Catalonia, Spain) and comparison with historical data.
2014
Through an extensive sampling in the Llobregat River basin, the presence of 50 currently used pesticides in water, sediment, and biota was assessed. Pesticides were detected primarily in water (up to 56% of the analytes), whereas their presence in sediments was more intermittent, and in biota was scarce. Those at high concentrations in water were the benzimidazoles (carbendazim in 22% of the samples up to 697ngL-1), the organophosphorus (malathion in 54% of the samples up to 320ngL-1), and the ureas (diuron in 54% of the samples up to 159ngL-1). However, this pattern differed in sediments and biota, which were contaminated primarily with organophosphorus (higher Kow) (chlorpyrifos 93% of se…
Last trends in pesticide residue determination by liquid chromatography–mass spectrometry
2014
Liquid chromatography–mass spectrometry (LC–MS) is as an excellent analytical tool in the determination of pesticides. Multiresidue analysis of these compounds at trace levels is one of the oldest analytical schemes within environmental and food safety. However, the issue of “pesticide residue determination” is still a hot topic for the analytical community. This review discusses current approaches and recent advances in using LC–MS for pesticide identification and quantification. We outline how MS has influenced the sample preparation process. We critically assess and compare various mass spectrometers, highlighting their strengths and limitations. We, then, review the main applications of…
Multiresidue analysis of organic pollutants by in-tube solid phase microextraction coupled to ultra-high performance liquid chromatography-electrospr…
2013
In this work, in-tube solid phase microextraction (IT-SPME) coupling with ultra-high-pressure liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) multiresidue analytical method has been proposed for the first time for on-line enrichment of 9 analytes included in Water Frame Directive 2000/60/EC (WFD). The device was equipped with a GC TRB-5 capillary column, used as pre-concentration loop, and two conventional six-port injection valves. Water sample and desorption solvent volumes were tested. The optimum conditions were 4mL of processed sample followed by elution with 40μL of methanol. The analytes were detected with a mass spectrometer after being ionized positively using an elect…
Pesticides in the Ebro River basin: Occurrence and risk assessment
2016
In this study, 50 pesticides were analyzed in the Ebro River basin in 2010 and 2011 to assess their impact in water, sediment and biota. A special emphasis was placed on the potential effects of both, individual pesticides and their mixtures, in three trophic levels (algae, daphnia and fish) using Risk Quotients (RQs) and Toxic Units (TUs) for water and sediments. Chlorpyrifos, diazinon and carbendazim were the most frequent in water (95, 95 and 70% of the samples, respectively). Imazalil (409.73 ng/L) and diuron (150 ng/L) were at the highest concentrations. Sediment and biota were less contaminated. Chlorpyrifos, diazinon and diclofenthion were the most frequent in sediments (82, 45 and 2…
Ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry to identify contaminants in water: an insight on environment…
2013
Ultra-high pressure liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-QqTOF-MS) acquiring full scan MS data for quantification, and automatic data dependent information product ion spectra (IDA-MS/MS) without any predefinition of the ions by the user was checked for identifying organic contaminants in water samples. The use of a database with more than 2000 compounds achieved high confidence results for a wide number of contaminants based upon retention time, accurate mass, isotopic pattern and MS/MS library searching. More than 20 contaminants, mostly pharmaceuticals, but also mycotoxins and polyphenols were unambiguously identified. Furthermore, the combination of s…
Analysis of insecticides in honey by liquid chromatography–ion trap-mass spectrometry: Comparison of different extraction procedures
2010
The feasibility of different extraction procedures was tested and compared for the determination of 12 organophosphorus and carbamates insecticides in honey samples. In this sense, once the samples were pre-treated - essentially dissolved in hot water by stirring - and before they could be analyzed by liquid chromatography-ion trap-second stage mass spectrometry (LC-MS(2)), four different approaches were studied for the extraction step: QuEChERS, solid-phase extraction (SPE), pressurized liquid extraction (PLE) and solid-phase microextraction (SPME). The main aim of this work was to maximise the sensitivity of pesticides and to minimise the presence of interfering compounds in the extract. …
Transcriptomic, biochemical and individual markers in transplanted Daphnia magna to characterize impacts in the field
2015
Daphnia magna individuals were transplanted across 12 sites from three Spanish river basins (Llobregat, Ebro, Jucar) showing different sources of pollution. Gene transcription, feeding and biochemical responses in the field were assessed and compared with those obtained in re-constituted water treatments spiked with organic eluates obtained from water samples collected at the same locations and sampling periods. Up to 166 trace contaminants were detected in water and classified by their mode of action into 45 groups that included metals, pharmaceuticals, pesticides, illicit drugs, and other industrial compounds. Physicochemical water parameters differentiated the three river basins with Llo…
Comparison of green sample preparation techniques in the analysis of pyrethrins and pyrethroids in baby food by liquid chromatography–tandem mass spe…
2017
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…
Perfluoroalkyl substance contamination of the Llobregat River ecosystem (Mediterranean area, NE Spain).
2014
The occurrence and sources of 21 perfluoroalkyl substances (PFASs: C4-C14, C16, C18 carboxylate, C4, C6-C8 and C10 sulfonates and C8 sulfonamide) were determined in water, sediment, and biota of the Llobregat River basin (NE Spain). Analytes were extracted by solid phase extraction (SPE) and determined by liquid chromatography triple quadrupole mass spectrometer (LC-QqQ-MS). All samples were contaminated with at least one PFAS, being the most frequently found perfluorobutanoate (PFBA), perfluorooctanoate (PFOA) and perfluorooctane sulfonate (L-PFOS). In general, mean PFAS concentrations measured in sediments (0.01-3.67 ng g(-1)) and biota (0.79-431 μg kg(-1)) samples were higher than those …