San Juan de la Rambla, Spain
San Juan de la Rambla, Spain

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El-Amrani S.,Complutense University of Madrid | Pena-Abaurrea M.,IQOG CSIC | Sanz-Landaluze J.,Complutense University of Madrid | Ramos L.,IQOG CSIC | And 2 more authors.
Science of the Total Environment | Year: 2012

The feasibility of a bioaccumulation test based on the use of zebrafish eleutheroembryos as an alternative to adult-individual-based approaches for REACH application has been evaluated for three test compounds, chlorpyrifos, dicofol and atrazine. Following the OECD 305 guidelines, zebrafish eleutheroembryos (72h after hatching, hpf) were separately exposed to the investigated pesticides at two nominal concentrations below 1% of its corresponding LC50. The uptake experiments lasted for 48h. Then, the exposure medium was replaced by a non-contaminated medium for depuration experiments (up to 72h). Zebrafish eleutheroembryos (larvae 144 hpf, i.e. at the end of the depuration step) and their corresponding exposure media was sampled at ten different times during each experiment and the concentration of the investigated pesticide determined in both the organisms and in the exposure medium. The experimentally determined pesticide accumulation profiles in the eleutheroembryos demonstrated that atrazine has a very fast accumulation kinetic, reaching steady sate (SS) within 24h. Chlorpyrifos and dicofol did not reach the SS within the 48-h uptake experiments although they exhibit higher accumulations than the former pesticide. Two toxicokinetic models were used to calculate the bioconcentration factor (BCF) of the studied pesticide in zebrafish eleutheroembryos. In the former, the BCF was calculated under SS conditions (BCFSS). The second was used when the compounds did not reach the SS during the uptake experiment (BCFk). Log BCF values of 3.55 and 3.84 for chlorpyrifos; 0.6 and 1.17 for atrazine, and 3.90 for dicofol were experimentally calculated at selected exposure concentrations. These values have been compared with those reported in related bioaccumulation studies and official databases. © 2012 Elsevier B.V.


Artiaga G.,Complutense University of Madrid | Ramos K.,Complutense University of Madrid | Ramos L.,IQOG CSIC | Camara C.,Complutense University of Madrid | Gomez-Gomez M.,Complutense University of Madrid
Food Chemistry | Year: 2015

In this work, silver migration from commercial food containers was evaluated according to European Regulation 10/2011. Several experimental parameters affected silver release: food simulant, temperature, exposition time and sampled bag area. Results demonstrated a significant silver nanoparticle (AgNP) migration into aqueous and acidic simulants. The amount of silver migrated increased with storage time and temperature although, in general, silver showed a low tendency to migrate into food simulants (17 ng/g). However, the food simulant did not seem to be a really outstanding variable for long term storage. AF4-ICP MS was used to confirm the presence of AgNPs in the simulants. The low limit of detection achieved (0.4 μg L-1) allowed the identification of AgNPs and their size characterisation (40-60 nm). Finally, scanning electron microscopy/energy-dispersive X-ray analysis suggested a possible transformation of the AgNPs detected in the extracts, due to association with other ligands, such as chlorine and sulphur, present in the original containers. © 2014 Elsevier Ltd. All rights reserved.


Gomara B.,IQOG CSIC. | Herrero L.,IQOG CSIC. | Pacepavicius G.,Environment Canada | Ohta S.,Setsunan University | And 2 more authors.
Chemosphere | Year: 2011

In this study, for the first time, levels and accumulation profiles of eight currently available polybrominated/chlorinated biphenyl congeners (PXBs; XB-77, -105, -118, -126A, -126B, -126C, -156 and -169, named according to IUPAC nomenclature) in human breast milk collected form Spanish women in 2005 were reported. Concentrations and congener specific profiles of polychlorinated biphenyls (PCBs), including co-planar PCBs, (co-PCBs) and polybrominated diphenyl ethers (PBDEs) were also reported.A concentration of 0.45pgg-1 lipid weight was found for total PXBs, and arithmetic mean concentrations of 125, 25 and 5.5ngg-1 lipid weight were determined for total PCBs, co-PCBs and total PBDEs respectively. Detectable levels of all congeners investigated, except CB-123 and XB-169 were found. Levels of PCBs were similar to those found in Spanish samples collected after 2000, and lower than those obtained before 2000. CB-138, -153 and -180 were the predominant PCB congeners. PBDE levels, dominated by BDE-47, -99, -100 and -209, were lower than PCB levels. PXB concentrations were the lowest, with XB-156 being the most abundant. The concentration levels of PCBs and PBDEs found in this study were in the same range as those from other European countries. Levels of PXBs were much lower than published values determined in Japan which were the only data found in the literature. © 2011 Elsevier Ltd.


Pena-Abaurrea M.,IQOG CSIC | Ye F.,Campus Management | Blasco J.,Campus Management | Ramos L.,IQOG CSIC
Journal of Chromatography A | Year: 2012

This study evaluates the feasibility of comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC × GC-ToF MS) for the determination of the 15. +. 1. EU PAHs in sediments. Experimental variables affecting the injection, chromatographic separation and analytical detection of the analytes have systematically been optimised. Under finally proposed conditions, a satisfactory resolution among critical pairs/groups of PAHs, including benz[. a]anthracene, cyclopenta[. cd]pyrene and chrysene, the three benzofluoranthene isomers, indeno[1,2,3. -cd]pyrene from dibenz[. a,. h]anthracene (DahA), and DahA from dibenz[. a,. c]anthracene, has been achieved using DB-5 × BPX-50 as column combination with a run time of 1. h. The feasibility of the method for the analysis of real-life samples has been demonstrated by accurate determination of relevant target PAHs in the certified harbour sediment BCR-535 (deviations among certified concentration values and those calculated using the proposed method lower than 3%); and by successful application to sediments sampled from a relevant protected area located in the South of Spain. The low methodological limits of detection (LODs) obtained for most of the targeted PAHs (in the 5.7-60 μg/kg range, as calculated for real samples) guarantied accurate quantification of the target compounds at the low levels expected in these types of pristine matrices. The strong retention experienced by the heaviest dibenzopyrene isomers included in the study resulted in relatively high LODs for these analytes; nevertheless, these compounds were detected at concentration levels above the corresponding LOD in some of the analysed sediments. In addition, the enhanced identification power provided by GC × GC-ToF MS for the identification of non-target analytes allowed the tentative identification of a group of polynuclear aromatic thiophenes in some of the test samples. Finally, the potential of the use of normalised bubble plots for the fast screening of the potential PAH sources has been demonstrated. © 2012 Elsevier B.V.


PubMed | IQOG CSIC and CSIC - Institute of Environmental Assessment And Water Research
Type: | Journal: Analytica chimica acta | Year: 2015

This paper reports on the optimisation, characterisation, validation and applicability of gas chromatography coupled to triple quadrupole mass spectrometry in its tandem operation mode (GC-QqQ(MS/MS) for the quantification of polychlorinated dibenzo-p-dioxins and furans (PCDD/Fs, dioxins) and dioxin-like polychlorinated biphenyls (DL-PCBs) in environmental and food matrices. MS/MS parameters were selected to achieve the high sensitivity and selectivity required for the analysis of this type of compounds and samples. Good repeatability for areas (RSD = 1-10%, for PCDD/Fs and DL-PCBs) and for ion transition ratios (RSD = 0.3-10%, for PCDD/Fs, and 0.2-15%, for DL-PCBs) and low instrumental limits of detection, 0.07-0.75 pg L(-1) (for dioxins) and 0.05-0.63 pg L(-1) (for DL-PCBs), were obtained. A comparative study of the congener specific determination using both GC-QqQ(MS/MS) and gas chromatography-high resolution mass spectrometry (GC-HRMS) was also performed by analysing several fortified samples and certified reference materials (CRMs) with low (feed and foodstuffs), median (sewage sludge) and high (fly ash) toxic equivalency (TEQ) concentration levels, i.e. 0.60, 1.83, 72.9 and 3609 pg WHO-TEQ(PCDD/Fs) g(-1). The agreement between the results obtained for the total TEQs (dioxins) on GC-QqQ(MS/MS) and GC-HRMS in all the investigated samples were within the range of 4%, and that of DL-PCBs at concentration levels of 0.84 pg WHO-TEQs (DL-PCBs) g(-1), in the case of feedstuffs, was 0.11%. Both instrumental methods have similar and comparable linearity, precision and accuracy. The GC-QqQ(MS/MS) sensitivity, lower than that of GC-HRMS, is good enough (iLODs in the down to low pg levels) to detect the normal concentrations of these compounds in food and environmental samples. These results make GC-QqQ(MS/MS) suitable for the quantitative analysis of dioxins and DL-PCBs and a real alternative tool to the reference sector HRMS instruments.


Pena-Abaurrea M.,IQOG CSIC | Covaci A.,University of Antwerp | Ramos L.,IQOG CSIC
Journal of Chromatography A | Year: 2011

This study evaluates comprehensive two-dimensional gas chromatography (GC × GC) coupled to time-of-flight mass spectrometry (GC × GC-ToF MS) for the simultaneous analysis of several classes of organobromines (OBs), including polybrominated diphenyl ethers (PBDEs), polybrominated biphenyls (PBBs), methoxylated PBDEs (MeO-PBDEs), several halogenated naturally produced compounds (HNPs) and eight novel brominated flame retardants (NBFRs), polybrominated hexahydroxanthene derivates (PBHDs), 2,4,6-tribromoanisole and a mixed halogenated compound (MHC-1), in bluefin tuna muscles. The proposed methodology maximised separation of both within and among OB families, and among these and other halogenated micropollutants detected in these samples and co-extracted matrix components. Special attention has been paid to solve co-elution problems observed during the analysis of OBs with one-dimensional GC-based techniques. Satisfactory separation among several relevant PBDEs and MeO-PBDEs has been obtained allowing their unambiguous determination in a single run. Additional studies were conducted to identify selected NBFRs and HNPs. 2,4-Dibromoanisole, a dibromophenol isomer and hexabromobenzene were identified in the investigated samples. Several new tri- and tetra-BHD derivates were also identified, indicating that these compounds could apparently exist as structured families in nature. In addition, a tetrabrominated diMeO-biphenyl and two tetrabrominated diMeO-BDEs were also tentatively identified. © 2011 Elsevier B.V.


Pena-Abaurrea M.,IQOG CSIC | Garcia de la Torre V.S.,IQOG CSIC | Ramos L.,IQOG CSIC
Journal of Chromatography A | Year: 2013

The use of solid-phase extraction pipette tip (also called disposable pipette extraction, DPX) has been evaluated for the purification of environmentally relevant polychlorinated biphenyls (PCBs) in fatty extracts obtained by ultrasound-assisted extraction with a sonication probe from small-size biological tissues. Complete sample treatment involved only 50. mg of sample and was completed in ca. 15. min with minimal sample manipulation and reagents consumption (i.e., 1.5. mL of n-hexane and 0.8. g of acidic silica). The performance of the proposed methodology for the intended determination was firstly evaluated by determination of the endogenous PCB levels in a naturally contaminated internal reference material. The determined concentrations showed a good agreement with those obtained using a more conventional sample preparation procedure previously validated in our laboratory (recoveries, as compared to levels determined using the latter method, were in the 85-123% range for a large majority of the studied congeners, and the relative standard deviations were in general lower than 14%). Results obtained for the analysis of reference food samples and certified reference materials NIST 1945 and 1947 demonstrated that, when combined with gas chromatography coupled to ion trap mass spectrometry working in the tandem mode, GC-ITD(MS/MS), the proposed methodology allowed accurate determination of most of the investigated PCBs and that 50. mg of sample sufficed for the screening of less abundant toxic congeners. © 2013 Elsevier B.V.


Ruiz-Aceituno L.,IQOG CSIC | Sanz M.L.,IQOG CSIC | Ramos L.,IQOG CSIC
TrAC - Trends in Analytical Chemistry | Year: 2013

This review highlights relevant advances in the use of ionic liquids (ILs) for analytical extraction and purification of organic compounds from food and environmental matrices.Following a technique-based structure, we discuss advantages and shortcomings of ILs compared to conventional volatile organic solvents. We focus on the use of ILs in modern miniaturized extraction techniques, highlighting recent trends. However, when relevant, we also consider more classical approaches to sample preparation.We discuss remaining limitations, gaps detected and possible future developments in this research area.Finally, we illustrate the feasibility of the several analytical procedures for the analysis of relevant organic and biomolecules in foodstuffs and environmental samples of different natures on the basis of representative studies of applications. © 2012 Elsevier Ltd.


Mohr S.,IQOG CSIC | Mohr S.,Federal University of Santa Maria | Mohr S.,CAPES Foundation | Garcia-Bermejo T.,IQOG CSIC | And 4 more authors.
Science of the Total Environment | Year: 2014

Concentrations of 17 brominated flame retardants (BFRs), including two "novel" BFRs (1,2-bis(2,4,6-tribromophenoxy)ethane, BTBPE and decabromodiphenylethane, DBDPE), have been determined to be in 35 commercial honey samples from Brazil, Spain, Portugal, Slovenia and Morocco. The results revealed the presence of low amounts (between


PubMed | IQOG CSIC and Federal University of Santa Maria
Type: | Journal: The Science of the total environment | Year: 2014

Concentrations of 17 brominated flame retardants (BFRs), including two novel BFRs (1,2-bis(2,4,6-tribromophenoxy)ethane, BTBPE and decabromodiphenylethane, DBDPE), have been determined to be in 35 commercial honey samples from Brazil, Spain, Portugal, Slovenia and Morocco. The results revealed the presence of low amounts (between

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