showing 44 related works from this author
Indoor air pesticide in dwellings of breastfeeding mothers of the Valencian Region (Spain): Levels, exposure and risk assessment
2021
This study assessed the inhalation risk associated with indoor pesticide concentrations in the dwellings of 41 lactating mothers living in the Valencian Region, Spain, who were participants in the BETTERMILK project. Twenty-eight substances were investigated, including pyrethroid (PYRs), organophosphate (OPPs), and organochlorine (OCPs) pesticides. Bifenthrin, cypermethrin, lambda-cyhalothrin, malathion, permethrin and pyrimethanil were detected with frequencies ranging from 2% (malathion) to 80% (cypermethrin), and with an arithmetic mean concentration ranging from 4.1 ng m(-3) (bifenthrin) to 12.1 ng m-(3) (cypermethrin). The indoor air analysis was combined with several surveys to assess…
Retrospective screening of pesticide metabolites in ambient air using liquid chromatography coupled to high-resolution mass spectrometry
2015
A new methodology for the retrospective screening of pesticide metabolites in ambient air was developed, using liquid chromatography coupled to Orbitrap high-resolution mass spectrometry (UHPLC-HRMS), including two systematic workflows (i) post-run target screening (suspect screening) and (ii) non-target screening. An accurate-mass database was built and used for the post-run screening analysis. The database contained 240 pesticide metabolites found in different matrixes such as air, soil, water, plants, animals and humans. For non-target analysis, a "fragmentation-degradation" relationship strategy was selected. The proposed methodology was applied to 31 air samples (PM10) collected in the…
Health Risk Assessment of Exposure to 15 Essential and Toxic Elements in Spanish Women of Reproductive Age: A Case Study
2021
This case study investigates the exposure of 119 Spanish women of reproductive age to 5 essential (Co, Cu, Mn, V, Zn) and 10 toxic (Ba, Be, Cs, Ni, Pb, Pt, Sb, Th, Al, U) elements and assesses their risk. The essential elements (Co, Cu, Mn, V, and Zn) showed average concentrations (GM: geometric mean) of 0.8, 35, 0.5, 0.2, and 347 μg/L, respectively. Five of the toxic elements (Ba, Cs, Ni, Al, U) exhibited detection frequencies of 100%. The GM concentrations of the novel toxic elements were 12 μg/L (Al), 0.01 μg/L (Pt), 0.02 μg/L (U), 0.12 μg/L (Th), 0.009 μg/L (Be) and 4 μg/L (Cs). The urine analysis was combined with a survey to assess any variations between subgroups…
Influence of diet in urinary levels of metals in a biomonitoring study of a child population of the Valencian region (Spain)
2018
[EN] Pollution by trace elements and its possible effect on organisms has become a worldwide concern due to the increasing presence of trace elements in the environment and especially in the food chain. Exposure to chemicals has traditionally been measured using environmental samples, however, human biomonitoring brings a different perspective, in which all sources and exposure pathways are integrated. The objective of this paper is to discern the possible relationship between children's diet and the metals found in children urine. With this aim in mind, a total of 120 voluntaries participated in a diet survey carried out in a school-aged population (age 6-11) from the Valencian region. In …
Indoor Air Quality including Respiratory Viruses
2021
The detection of SARS-CoV-2 in indoor environments is a cause of increasing concern. In this study, three sampling methodologies have been used in order to collect SARS-CoV-2 and 17 other respiratory viruses in indoor air, combined with a new analytical process to analyze respiratory viruses. Different areas of an ophthalmological hospital were investigated for the presence of these airborne viruses. Moreover, indoor air quality (IAQ) parameters (carbon dioxide, CO2; carbon monoxide, CO; nitrogen dioxide, NO2; volatile organic compounds, VOCs; formaldehyde, HCHO; and particulate matter, PM) have been examined to study the relationship between IAQ and airborne viruses. All indoor air and sur…
Determination of 40 currently used pesticides in airborne particulate matter (PM 10) by microwave-assisted extraction and gas chromatography coupled …
2011
A confirmatory and sensitive procedure has been developed for the determination of 40 currently used pesticides (Cups) in airborne particulate matter (PM 10) at trace level. The proposed method includes extraction of PM 10-bound pesticides by microwave-assisted extraction (MAE) followed by a gel permeation chromatography (GPC) clean-up and determination by GC-MS/MS. The injection mode and the main parameters in MS/MS were optimized. The matrix effect was also evaluated. Recoveries ranged from 70 to 120% except for pyrimethanil and pirimicarb. The limit of quantification (LOQ) ranged from 1.32 to 39.47 pg m(-3), when air volumes of 760 m(3) were collected. The method was applied to 38 sample…
Analysis of four parabens and bisphenols A, F, S in urine, using dilute and shoot and liquid chromatography coupled to mass spectrometry
2018
Abstract A new strategy for the analysis of 4 parabens (methylparaben, ethyl paraben, propyl paraben and butyl paraben) and 3 bisphenols (A, F and S) in human urine has been developed. Dilute and shoot and liquid chromatography coupled to mass spectrometry (LC-MS/MS) determination was employed. Procedural matched calibration, certified materials and spiked samples were used for validation. The obtained recoveries varied between 85 and 104% with a precision lower than 20% for all analytes. The LOQ was 0.20 ng mL for all analytes. Negative atmospheric pressure chemical ionization in the selected reaction monitoring mode was used for MS detection. The proposed method was successfully applied f…
Pesticide Inhalation Exposure of Applicators and Bystanders Using Conventional and Innovative Cropping Systems in the Valencian Region, Spain
2021
This paper provides scientific results from a European LIFE project carried out in the Valencian region of Spain during the 2017 to 2018 time frame. In 2018, more than 60,000 tons of pesticides were commercialized in Spain, with approximately 15% destined for Valencian crops. In order to improve the air quality in the agricultural areas of this region, an innovative cropping system based on irrigation was developed and compared to conventional treatments based on hand-spray and turbo application. After applying conventional treatments to five types of crops (citrus, persimmon, nectarine, watermelon, and other stone fruits), a total of 13 active substances were detected in the air. The same …
Risk assessment of exposure to phthalates in breastfeeding women using human biomonitoring
2020
In this study, we assessed the presence of 14 phthalate metabolites in the urine of 104 lactating mothers from Valencia (Spain) who took part in the human biomonitoring project BETTERMILK. Nine of the metabolites studied showed detection frequencies >80%, whereas the rest of the metabolites presented low detection frequencies (<5%). The concentrations ranged from <LoQ to 1291 ng/mL with monoethyl phthalate showing the highest concentration, with a geometric mean of 34.90 ng/mL. In general, the phthalate metabolite levels quantified in the present study were lower than the urinary levels found in previous studies that involved lactating mothers. The consumption of packaged juices and the fre…
New screening approach for risk assessment of pesticides in ambient air
2014
We present a novel screening approach for inhalation risk assessment of currently used pesticides (CUPs) in ambient air, based on the measurements of pesticide levels in the inhalable fraction of the particulate matter (PM10). Total concentrations in ambient air (gas + particle phases) were estimated using a theoretical model of distribution of semi-volatile organic compounds between the gas and the particulate phase based on the octanol-air partition (K-oa) of each pesticide. The proposed approach was used in a pilot study conducted in a rural station in Valencia (Spain) from April through to October 2010. Twenty out of 82 analysed pesticides were detected in average concentrations ranging…
Quick determination of Glyphosate and AMPA at sub µg/L in drinking water by direct injection into LC-MS/MS
2021
Abstract A sensitive, simple and quick method for the determination of glyphosate (Gly) and its degradation product, Aminomethyl phosphonic acid (AMPA), in water through ion chromatography coupled to quadrupole-linear ion trap mass spectrometry has been developed. Sample treatment was based on direct injection and acquisition was implemented in both MS2 and MS3 modes. The LoQs of the method were 0.03 µ/L for both Gly-and AMPA. The recoveries were between 91 and 118% and RSD was lower than 15%. The developed methodology was applied on 436 water samples.
Occurrence of biomarkers of pesticide exposure in non-invasive human specimens.
2015
Biomonitoring has been used in many types of investigations, including national programmes and epidemiological studies, to explore the occurrence of biomarkers of pesticide exposure in the general population or relevant groups. This review discusses recent studies that measure levels of biomarkers of pesticide exposure in non-invasive human specimens such as urine, breast milk, meconium and hair. Specific and non-specific metabolites of organophosphate and pyrethroid insecticides have been widely investigated in urine, where some of the suitable biomarkers present rates of detection higher than 80%, which stand for an ongoing chronic exposure to traces of these chemicals. Hair is a promisin…
Exposure and Risk Assessment of Hg, Cd, As, Tl, Se, and Mo in Women of Reproductive Age Using Urinary Biomonitoring
2021
The present study analyzed the exposure and risk assessment of 4 toxic (Hg, Cd, As, Tl) and 2 essential (Se, Mo) elements in 119 Spanish women of reproductive age. The focus was on the elements for which risk-based benchmark, biomonitoring equivalents, or health-related human biomonitoring values have already been established. All elements presented frequencies of detection of 100% (greater than the limit of detection), except for Cd (99%). The 95th percentile concentrations were, for the toxic metals, 358.37 µg/L (total As), 1.10 µg/L (Cd), 0.41 µg/L (Tl), and 3.03 µg/L (total Hg) and, for the essential elements, 68.95 µg/L (total Se) and 154.67 (Mo). We examined sociodemographic factors a…
Determination of 60 Migrant Substances in Plastic Food Contact Materials by Vortex-Assisted Liquid-Liquid Extraction and GC-Q-Orbitrap HRMS
2021
A GC-HRMS analytical method for the determination of 60 migrant substances, including aldehydes, ketones, phthalates and other plasticizers, phenol derivatives, acrylates, and methacrylates, in plastic food contact materials (FCM) has been developed and validated. The proposed method includes migration tests, according to Commission Regulation (EU) 10/2011, using four food simulants (A, B, C, and D1), followed by vortex-assisted liquid–liquid extraction (VA-LLE) and GC-Q-Orbitrap HRMS analysis in selected ion monitoring (SIM) mode, with a resolving power of 30,000 FWHM and a mass accuracy ≤5 ppm. The method was validated, showing satisfactory linearity (R2 ≥ 0.98 from 40 to 400 …
Biomonitoring of polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs) and dioxin-like polychlorinated biphenyls (dl-PCBs)…
2020
Abstract The main objective of the present research was to evaluate the levels of polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs), and dioxin-like polychlorinated biphenyls (dl-PCBs) in the human milk of Spanish lactating women who participated in the BETTERMILK project so that exposure and risk could be assessed for these mothers and their breastfed children. The total ∑PCDD/Fs + dl-PCBs TEQ2005 concentrations in the upper-bound (UB) ranged from 1.29 to 13.48 pg TEQ2005 g−1 lipid. The estimated geometric mean level for the sum of PCDD/F and dl-PCBs was 4.10 and 4.42 pg TEQ2005 g−1 lipid, lower-bound (LB) and UB respectively and were below the reference leve…
Combined target and post-run target strategy for a comprehensive analysis of pesticides in ambient air using liquid chromatography-Orbitrap high reso…
2014
Abstract A comprehensive strategy for the analysis of current airborne pesticides has been developed using liquid chromatography coupled to high resolution mass spectrometry. The methodology includes both quantitative target analysis and post-run target screening analysis. The quantitative method was validated after a previous statistical optimisation of the main factors governing the ion source ionization and a study of the single-stage Orbitrap fragmentation through the HCD cell. The quantitative method presented recoveries ranging from 73 to 116%, with precision (RSD) lower than 20%, for the 35 substances in the scope of the target method. The full-scan accurate mass data were acquired w…
Particle size distributions of currently used pesticides in ambient air of an agricultural Mediterranean area
2014
This work presents first data on the particle size distribution of 16 pesticides currently used in Mediterranean agriculture in the atmosphere. Particulate matter air samples were collected using a cascade impactor distributed into four size fractions in a rural site of Valencia Region, during July to September in 2012 and from May to. July in 2013. A total of 16 pesticides were detected, including six fungicides, seven insecticides and three herbicides. The total concentrations in the particulate phase (TSP: Total Suspended Particulate) ranged from 3.5 to 383.1 pg m(-3). Most of the pesticides (such as carbendazim, tebuconazole, chlorpyrifos-ethyl and chlorpyrifos-methyl) were accumulated …
Biomonitoring of Phthalates, Bisphenols and Parabens in Children: Exposure, Predictors and Risk Assessment
2021
Exposure to emerging contaminants, such as phthalates, bisphenols and parabens in children has been associated with possible neurodevelopment and endocrine alterations. In the present study, the biomonitoring of biomarkers in children (5–12 years old) from the Valencia Region (Spain) have been implemented using urines from the BIOVAL program. More than 75% of the children studied (n = 562) were internally exposed (>
Utilization of long duration high-volume sampling coupled to SPME-GC-MS/MS for the assessment of airborne pesticides variability in an urban area (St…
2016
Atmospheric samples have been collected between 14 March and 12 September 2012 on a 2-week basis (15 days of sampling and exchange of traps each 7 days) in Strasbourg (east of France) for the analysis of 43 pesticides. Samples (particle and gas phases) were separately extracted using Accelerated Solvent Extraction (ASE) and pre-concentrated by Solid Phase Micro-Extraction (SPME) before analysis by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS). Four SPME consecutive injections at distinct temperatures were made in order to increase the sensitivity of detection for the all monitored pesticides. Currently used detected pesticides can be grouped in four classes; those used i…
Optimization of Resolving Power, Fragmentation, and Mass Calibration in an Orbitrap Spectrometer for Analysis of 24 Pesticide Metabolites in Urine
2019
Mass spectrometer parameters such as Resolving Power, type of fragmentation, and mass calibration mode were optimized in the analysis of 24 pesticide metabolites in human urine using Ultra-High Pressure Liquid Chromatography coupled to Orbitrap High-Resolution Mass Spectrometer (UHPLC-HRMS). The best results were achieved with a Resolving Power of 25,000 FWHM and by applying Collision Induced Dissociation fragmentation mode (40 eV).
Evaluation of sampling adsorbents and validation of a LC-HRMS method for determination of 28 airborne pesticides
2018
A new strategy for sampling, using a low-volume sampler, and determination of airborne pesticides by liquid chromatography coupled to high-resolution mass spectrometry (UHPLC-HRMS) has been developed. The trapping efficiency of three adsorbents (sandwich PUF-XAD2-PUF; XAD-2 and XAD-4) was tested for 33 currently used pesticides and the first adsorbent (PUF-XAD2-PUF) was selected because it presented the highest retention capacity without breakthrough. Selected PUF-XAD2-PUF had the following design: 5 g of Amberlite XAD-2 sandwiched between two cylinders of PUF (6.87 cm(3), height: 1.4 cm, diameter: 2.5 cm). A validation of the analytical methodology that includes microwave extraction with e…
Multi-residue analysis of 30 currently used pesticides in fine airborne particulate matter (PM 2.5) by microwave-assisted extraction and liquid chrom…
2009
A confirmatory and rapid procedure has been developed for the determination of 30 currently used pesticides (CUP) in fine airborne particulate matter (PM 2.5) at trace level. The proposed method includes extraction of PM 2.5-bound pesticides by microwave-assisted extraction (MAE) followed by a direct injection into LC-MS/MS. The main parameters affecting the MAE extraction (time, temperature and volume of solvent) were optimised using statistical design of experiments (DoE). The matrix effect was also evaluated. Recoveries ranged from 72 to 109% and the limit of quantification (LoQ) was 32.5 pg m(-3) for chlorpyrifos, 13.5 pg m(-3) for fenhexamid, imazalil and prochloraz, and 6.5 pg m(-3) f…
Biomonitoring of bisphenols A, F, S and parabens in urine of breastfeeding mothers: Exposure and risk assessment
2019
In the present study we used human biomonitoring to assess the internal exposure and the risk to four parabens and three bisphenols in 103 Spanish breastfeeding mothers participating in the BETTERMIILK project. Urinary methylparaben (MP), ethylparaben (EP), propylparaben (PP) and butylparaben (BP) presented detection frequencies ranging from 12% (BP) to 92% (MP), while bisphenol A (BPA), bisphenol F (BPF) and bisphenol S (BPS) were detected in 76% (BPA) and 20% (BPF, BPS) of the mothers. Average paraben concentrations (geometric mean) ranged from 0.021 ng mL(-1) (BP) to 17.7 ng mL(-1) (MP), whereas bisphenols had geometric means concentrations from 0.042 ng mL(-1) (BPF) to 0.927 ng mL(-1) (…
GC–MS characterization of contemporary pesticides in PM10 of Valencia Region, Spain
2012
Pesticides in the inhalable fraction of particulate matter (PM10) should be well tracked in order to contribute information to future exposure assessment in individuals of the general public. A total of 40 current-used pesticides and metabolites were searched for in ambient air samples collected from January through December 2010. The samples were taken from one remote, one urban and three rural sites in Valencia Region (Spain) and analyzed using liquid chromatography coupled to mass spectrometry in tandem (LC-MS/MS). In the PM10 fraction 17 pesticides and metabolites were detected overall, two of them currently banned (carbofuran and omethoate, although the latter is a metabolite of the pe…
Particle size distributions of currently used pesticides in a rural atmosphere of France
2013
This work presents first data on the particle size distributions of current-used pesticides in the atmosphere. Ambient air samples were collected using a cascade impactor distributed into four size fractions in a rural site of Centre Region (France). Most pesticides were accumulated in the fine (0.1-1 mu m) particle size fraction such as cyprodinil, pendimethalin, fenpropidin, fenpropimorph and spiroxamine. Other pesticides such as acetochlor and metolachlor presented a bimodal distribution with maximum concentrations in the ultrafine (0.03-0.1 mu m) coarse (1-10 mu m) and in the ultrafine fine size ranges, respectively. No pesticides were detected in the size fraction >10 mu m. (C) 2013 El…
Biomonitoring of mercury in hair of breastfeeding mothers living in the Valencian Region (Spain). Levels and predictors of exposure
2017
This study focused on the evaluation of the levels of total mercury in hair among 120 breastfeeding mothers aged 20 to 45-. The concentrations of Hg ranged from 0.07 to 6.87 mu g/g with a geometric mean (GM) of 1.22 mu g/g. This GM is six times higher than the average internal exposure of mothers from other 17 European countries (0.225 mu g/g). Near 70% of mothers presented levels of Hg above the USA EPA internal exposure guideline of 1 mu g/g, and 27% exceeded the EFSA health-based guidance value of 1.9 mu g/g. The multivariate regression analysis revealed that age, smoking and fish consumption (sword fish, small fat fish, small lean fish) were the major predictors of mercury in hair. (C) …
Retrospective analysis of pesticide metabolites in urine using liquid chromatography coupled to high-resolution mass spectrometry
2016
Abstract A comprehensive retrospective analysis of pesticide metabolites in urine was developed, using liquid chromatography coupled to Orbitrap high-resolution mass spectrometry (UHPLC-HRMS) that includes both post-run target (suspect screening) and non-target screening. An accurate-mass database comprising 263 pesticide metabolites was built and used for the post-run screening analysis. For non-target analysis, a “fragmentation-degradation” relationship strategy was selected. The proposed methodology was applied to 49 real urine samples from pregnant women. In the post-target analysis 26 pesticide metabolites were tentatively identified, 8 of which (2-diethylamino-6-methyl-pyrimidinol; 3-…
Analysis of currently used pesticides in fine airborne particulate matter (PM 2.5) by pressurized liquid extraction and liquid chromatography-tandem …
2008
During and after the application of currently used pesticides (CUPs) a significant fraction of applied pesticides can be lost to the air. A confirmatory and rapid procedure has been developed for the determination of four fungicides (carbendazim, thiabendazol, imazalil and bitertanol), three insecticides (imidacloprid, methidathion and pyriproxyfen), one helicide (methiocarb) and one acaricide (hexythiazox) in fine airborne particulate matter (PM 2.5) at trace level. The proposed method includes extraction of PM 2.5-bound pesticides by pressurized liquid extraction (PLE) followed by a direct injection into LC-MS/MS. The main parameters affecting the performance of the electrospray ionizatio…
Human Biomonitoring of food contaminants in Spanish children: Design, sampling and lessons learned
2017
Abstract Human Biomonitoring (HBM) studies are highly useful for evaluating population exposure to environmental contaminants and are being carried out in increasing numbers all over the world. The use of HBM in the field of food safety, in a risk assessment context, presents a growing interest as more health-based guidance values (HBGV) in biological matrices are derived, and can be used in a complementary way to the external exposure approaches such as total diet studies or surveillance programmes. The aims of the present work are: i) to describe the methodological framework of the BIOVAL study, a cross-sectional HBM program carried out by the Health Department of the Regional Government …
Analytical methods for human biomonitoring of pesticides. A review.
2015
Biomonitoring of both currently-used and banned-persistent pesticides is a very useful tool for assessing human exposure to these chemicals. In this review, we present current approaches and recent advances in the analytical methods for determining the biomarkers of exposure to pesticides in the most commonly used specimens, such as blood, urine, and breast milk, and in emerging non-invasive matrices such as hair and meconium. We critically discuss the main applications for sample treatment, and the instrumental techniques currently used to determine the most relevant pesticide biomarkers. We finally look at the future trends in this field.
Occurrence of currently used pesticides in ambient air of Centre Region (France)
2010
Ambient air samples were collected, from 2006 to 2008 at three rural and two urban sites in Centre Region (France) and analyzed for 56 currently used pesticides (CUPS), of which 41 were detected. The four CUPs most frequently detected were the herbicides trifluralin, acetochlor and pendimethalin and the fungicide chlorothalonil, which were found with frequencies ranging between 52 and 78%, and with average concentrations of 1.93, 1.32, 1.84 and 12.15 ng m(-3), respectively. Among the detected pesticides, concentrations of eight fungicides (spiroxamine, fenpropimorph, cyprodinil, tolyfluanid, epoxiconazole, vinchlozolin, fluazinam, fludioxinil), two insecticides (propargite, ethoprophos), an…
Exposure to non-persistent pesticides in the Spanish population using biomonitoring: A review
2021
Abstract Although Spain does not have a regular national human biomonitoring program yet, different research groups are active in evaluating the exposure of children and adults to chemicals. In the last seven years, several studies in Spain have evaluated the internal exposure of the population to currently used pesticides. The present review analyzes the scope of these studies, the employed analytical methods and the main results of the exposure and risk, mainly for children and mothers. The frequency of exposure to biomarkers of exposure to organophosphate pesticides is high. Some non-specific dialkyl phosphate metabolites (DAPs), such as the diethyl phosphate (DEP), present Detection Fre…
Exposure assessment of Spanish lactating mothers to acrylamide via human biomonitoring.
2021
Abstract Acrylamide (AA) is an organic compound classified as “Probably carcinogenic to humans” (Group 2 A) that can be found principally in processed carbohydrate-rich foods and tobacco smoke. In humans, after exposure, AA is rapidly metabolized and excreted in urine, predominantly as N-acetyl-S-(2-carbamoylethyl)-l-cysteine (AAMA), N-acetyl-S-(2-carbamoyl-2-hydroxyethyl)-l-cysteine (GAMA3) and N-Acetyl-3-[(3-amino-3-oxopropyl)sulfinyl]-L-alanine (AAMA-Sul), which can be used as short-term biomarkers of exposure to AA. In this study, the presence of AA metabolites in urine samples of lactating mothers living in Spain (n = 114) was analyzed by “dilute and shoot” and liquid chromatography co…
Determination of acrylamide in coffee and chocolate by pressurised fluid extraction and liquid chromatography-tandem mass spectrometry.
2007
A selective and sensitive procedure has been developed and validated for the determination of acrylamide in difficult matrices, such as coffee and chocolate. The proposed method includes pressurised fluid extraction (PFE) with acetonitrile, florisil clean-up purification inside the PFE extraction cell and detection by liquid chromatography (LC) coupled to atmospheric pressure ionisation in positive mode tandem mass spectrometry (APCI-MS-MS). Comparison of ionisation sources (atmospheric pressure chemical ionisation (APCI), atmospheric pressure photoionization (APPI) and the combined APCI/APPI) and clean-up procedures were carried out to improve the analytical signal. The main parameters aff…
Comprehensive analysis of photoinitiators and primary aromatic amines in food contact materials using liquid chromatography High-Resolution Mass Spec…
2018
Abstract A comprehensive strategy for the analysis of UV-ink photoinitiators and primary aromatic amines (PAAS) in food-packaging materials such as, juice tetrabricks, pouches and bags has been developed using liquid chromatography coupled to Orbitrap High-Resolution Mass Spectrometry (LC-Orbitrap-HRMS). The methodology includes both quantitative target analysis and post-run target screening analysis. The quantitative method was validated after a previous optimisation of the single-stage Orbitrap fragmentation through the Higher-Energy Collisional Dissociation (HCD) Cell. Overall, the quantitative method presented recoveries ranging from 78% to 119%, with a precision (RSD) lower than 20%, f…
Analytical strategies for organic food packaging contaminants
2016
In this review, we present current approaches in the analysis of food-packaging contaminants. Gas and liquid chromatography coupled to mass spectrometry detection have been widely used in the analysis of some relevant families of these compounds such as primary aromatic amines, bisphenol A, bisphenol A diglycidyl ether and related compounds, UV-ink photoinitiators, perfluorinated compounds, phthalates and non-intentionally added substances. Main applications for sample treatment and different types of food-contact material migration studies have been also discussed. Pressurized Liquid Extraction, Solid-Phase Microextraction, Focused Ultrasound Solid-Liquid Extraction and Quechers have been …
Liquid chromatography‐Orbitrap Tribrid high‐resolution mass spectrometry using data dependent‐tandem mass spectrometry with triple stage fragmentatio…
2021
A new, fast, and automatic approach has been applied for the tentative identification of unknown substances released by food contact epoxy resin after performing a migration test with food simulant. This approach combines intelligent data acquisition with AcquireX linked to liquid chromatography-Orbitrap Tribrid high-resolution mass spectrometry using data dependent-tandem mass spectrometry with triple stage fragmentation coupled to Compound Discoverer™ software for automated data processing and compound identification. The identification of the observed features was performed using a set of identification criteria, including exact mass, isotope pattern, tandem mass spectrometry spectra mat…
Sampling and analysis of pesticides in ambient air.
2008
Developments in the sampling and determination of pesticides in ambient air have been discussed and data on the occurrence of pesticides in atmosphere have been presented. Developments in active sampling methods were reviewed and the different materials used for trapping pesticides from gas and particulate phases were discussed. Likewise, the use and developments of passive air samplers were reviewed. This article pays special attention to the analysis of pesticides trapped from ambient air, and recapitulate the procedures for extraction, clean-up and determination of these substances. Improvements in sampling procedures, analytical methods and monitoring activities are necessary to advance…
Biomonitoring of glyphosate and AMPA in the urine of Spanish lactating mothers
2021
The objectives of this study were to evaluate the urinary levels of Glyphosate (Gly) and its metabolite aminomethylphosphonic acid (AMPA) in Spanish breastfeeding mothers (n = 97), to identify the main predictors of exposure and to perform a risk assessment. Urine samples were analyzed using a method based on solid phase extraction and liquid chromatography tandem mass spectrometry (LC-MS/MS) determination. The developed method showed limits of quantification of 0.1 μg/L for both analytes. The detection frequencies (DFs) were 54% for Gly and 60% for AMPA, with geometric means (GMs) of 0.12 μg/L and 0.14 μg/L, respectively. In the statistical analysis, no relationship was found between the u…
Selection of sampling adsorbents and optimisation and validation of a GC-MS/MS method for airborne pesticides
2017
ABSTRACTA methodology for the sampling and determination of airborne pesticides has been developed. The trapping efficiency of three adsorbents, namely XAD-2,XAD-4 and a sandwich sorbent (PUF-XAD2-PUF), was tested for 34 pesticides and the latter was selected because it presented the highest retention capacity without breakthrough. Pesticides were determined by gas chromatography coupled to an ion trap mass spectrometer in tandem. The method showed recoveries ranging from 70% to 120% with limits of quantification in the range of 16.1–322.6 pg m−3 when 155 m3 were sampled. This analytical strategy was applied to 10 indoor air samples collected in dwellings from the Valencian Region. Six pest…
Methodological Aspects for the Implementation of the Air Pesticide Control and Surveillance Network (PESTNet) of the Valencian Region (Spain)
2021
A large amount of pesticide, applied mainly during agricultural practice, is released into the atmosphere, decreasing air quality and potentially causing public health problems. The Valencian region, after Andalusia, is the Spanish region with the highest consumption of pesticides owing to its large areas of agricultural land and the existence of crops that require intensive use of pesticides. In this work, we describe the sampling and analytical tools developed in the last decade and their transference to the Regional Department for Environment, where the main objective of the research was the creation and implementation of an Air pesticide control and surveillance network (PESTNet) in the…
Comprehensive analysis of airborne pesticides using hard cap espresso extraction-liquid chromatography-high-resolution mass spectrometry
2017
A hard cap espresso extraction procedure has been developed to recover airborne pesticides in particulate matter trapped in filters. This extraction step was made for 20s at 72°C and 19bar using 50mL of 20% (v/v) acetonitrile in water. After that, based on NaCl salting out, extracts were concentrated 22 times and analysed by ultra-high performance liquid chromatography - high resolution mass spectrometry. 35 pesticides were evaluated, as a proof of concept, being validated the whole methodology and compared the extraction method with that based on microwave assisted extraction for 20min. In short, the method avoids cross-contamination of samples, it is relatively fast and consumes only 10mL…
Human exposure and risk assessment to airborne pesticides in a rural French community
2016
Abstract Outdoor air samples collected during the pesticide agricultural application period (spring and summer) from a rural community in the Centre Region (France) were analyzed to investigate temporal variation of atmospheric pesticide levels (2006–2013) and human inhalation exposure in adults, children and infants. The most frequently detected pesticides were herbicides (trifluralin, pendimethalin), fungicides (chlorothalonil) and insecticides (lindane and α-endosulfan). The three currently-used pesticides most frequently detected presented concentrations ranging from 0.18 to 1128.38 ng m − 3 ; 0.13 to 117.32 ng m − 3 and 0.16 to 25.80 ng m − 3 for chlorothalonil, pendimethalin and trifl…
Target analysis of primary aromatic amines combined with a comprehensive screening of migrating substances in kitchen utensils by liquid chromatograp…
2015
An analytical strategy including both the quantitative target analysis of 8 regulated primary aromatic amines (PAAs), as well as a comprehensive post-run target screening of 77 migrating substances, was developed for nylon utensils, using liquid chromatography-orbitrap-high resolution mass spectrometry (LC-HRMS) operating in full scan mode. The accurate mass data were acquired with a resolving power of 50,000 FWHM (scan speed, 2 Hz), and by alternating two acquisition events, ESI+ with and without fragmentation. The target method was validated after statistical optimization of the main ionization and fragmentation parameters. The quantitative method presented appropriate performance to be u…