32 results on '"Marín-Sáez J"'
Search Results
2. P25-21 Examining the impact of a realistic mixture of dietary contaminants on the intestinal barrier and compounds absorption
- Author
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Araújo, A., Ramos, H., Ribeiro, M., Martins, Z., Marín-Sáez, J., Lopez-Ruiz, R., Faria, M., and Ferreira, I.
- Published
- 2024
- Full Text
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3. Stacked volume holographic gratings for extending the operational wavelength range in LED and solar applications
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Keshri, S., primary, Marín-Sáez, J., additional, Naydenova, I., additional, Murphy, K., additional, Atencia, J., additional, Chemisana, D., additional, Garner, S., additional, Collados, M. V., additional, and Martin, S., additional
- Published
- 2020
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4. Resonance ionization spectroscopy of sodium Rydberg levels using difference frequency generation of high-repetition-rate pulsed Ti:sapphire lasers
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Naubereit, P., primary, Marín-Sáez, J., additional, Schneider, F., additional, Hakimi, A., additional, Franzmann, M., additional, Kron, T., additional, Richter, S., additional, and Wendt, K., additional
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- 2016
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5. Holographic Photovoltaic-Thermal Module for Window Louvre Integration: Design and Simulation
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Chemisana, Daniel, primary, Marín-Sáez, J, additional, Riverola, A, additional, Moreno, A, additional, Atencia, J, additional, and Collados, M V, additional
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- 2016
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6. White-light optical vortices generated with holographic optical elements.
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Marín-Sáez, J., Collados, M. V., Sola, I. J., and Atencia, J.
- Abstract
A photograph of a white-light vortex obtained by means of volume phase holographic optical elements that allow creating achromatic vortices for a wide spectral range is shown. The elements have been recorded in dichromated gelatin and have a high damage threshold, so they are suitable for the generation of optical vortices with ultraintense femtosecond laser pulses. [ABSTRACT FROM AUTHOR]
- Published
- 2015
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7. A comprehensive study on the digestion, absorption, and metabolization of tropane alkaloids in human cell models.
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Marín-Sáez J, Lopez-Ruiz R, Faria MA, Ferreira IMPLVO, and Garrido Frenich A
- Subjects
- Humans, Digestion, Tea metabolism, Tea chemistry, Alkaloids metabolism, Tropanes metabolism
- Abstract
Tropane alkaloids (TAs) are toxic compounds with potent anticholinergic effects. Herbal infusions are among the most contaminated food commodities; however, the fate of TAs after ingestion remains poorly understood. This study presents a comprehensive investigation into the absorption, and metabolism of five TAs (atropine, scopolamine, tropine, homatropine, and apoatropine) following the digestion of contaminated tea. In vitro human cell models were employed, including gastric (NCI-N87), intestinal (Caco-2:HT29-MTX), and hepatic (HEP-G2) cells. TAs were found to be highly absorbed in the intestinal epithelium, while gastric cells exhibited poor absorption. Metabolism was studied using a custom-made database, revealing that it occurs predominantly in intestinal cells, involving hydroxylation and methylation reactions. Cell metabolomics was conducted using annotation, fragment simulation, and statistical software platforms. Significant statistical differences were observed for 40 tentatively identified compounds. MetaboAnalyst 5.0 was employed to discern the most disturbed metabolic pathways, with amoniacids biosynthesis pathways and TCA cycles being the most affected. These pathways are involved in responses to cellular metabolic stress, neurotransmitter production, cellular energy generation, and the regulation of oxidative stress response. The findings of this study enhance our understanding of the fate of TAs after ingestion, their metabolization and their effects at the cellular level., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)
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- 2024
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8. Analytical challenges and opportunities in the study of endocrine disrupting chemicals within an exposomics framework.
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Marín-Sáez J, Hernández-Mesa M, Cano-Sancho G, and García-Campaña AM
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- Humans, Environmental Exposure analysis, Endocrine Disruptors analysis, Exposome
- Abstract
Exposomics aims to measure human exposures throughout the lifespan and the changes they produce in the human body. Exposome-scale studies have significant potential to understand the interplay of environmental factors with complex multifactorial diseases widespread in our society and whose origin remain unclear. In this framework, the study of the chemical exposome aims to cover all chemical exposures and their effects in human health but, today, this goal still seems unfeasible or at least very challenging, which makes the exposome for now only a concept. Furthermore, the study of the chemical exposome faces several methodological challenges such as moving from specific targeted methodologies towards high-throughput multitargeted and non-targeted approaches, guaranteeing the availability and quality of biological samples to obtain quality analytical data, standardization of applied analytical methodologies, as well as the statistical assignment of increasingly complex datasets, or the identification of (un)known analytes. This review discusses the various steps involved in applying the exposome concept from an analytical perspective. It provides an overview of the wide variety of existing analytical methods and instruments, highlighting their complementarity to develop combined analytical strategies to advance towards the chemical exposome characterization. In addition, this review focuses on endocrine disrupting chemicals (EDCs) to show how studying even a minor part of the chemical exposome represents a great challenge. Analytical strategies applied in an exposomics context have shown great potential to elucidate the role of EDCs in health outcomes. However, translating innovative methods into etiological research and chemical risk assessment will require a multidisciplinary effort. Unlike other review articles focused on exposomics, this review offers a holistic view from the perspective of analytical chemistry and discuss the entire analytical workflow to finally obtain valuable results., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 The Authors. Published by Elsevier B.V. All rights reserved.)
- Published
- 2024
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9. Simultaneous detection of mycotoxins and pesticides in human urine samples: A 24-h diet intervention study comparing conventional and organic diets in Spain.
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Gallardo-Ramos JA, Marín-Sáez J, Sanchis V, Gámiz-Gracia L, García-Campaña AM, Hernández-Mesa M, and Cano-Sancho G
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- Humans, Male, Adult, Spain, Female, Pilot Projects, Food, Organic, Food Contamination analysis, Diet, Biological Monitoring methods, Young Adult, Middle Aged, Mycotoxins urine, Pesticides urine
- Abstract
Pesticides and mycotoxins, prominent chemical hazards in the food chain, are commonly found in plant-based foods, contributing to their pervasive presence in the human body, as evidenced by biomonitoring programs. Despite this, there is limited knowledge about their co-occurrence patterns. While intervention studies have demonstrated that organic diets can significantly reduce pesticide levels, their impact on mycotoxin exposure has been overlooked. To address this gap, this study pursued two objectives: first, to characterize the simultaneous presence of mycotoxins and pesticides in human urine samples by means of the control of the biomarkers of exposure, and second, to investigate the influence of consuming organic foods on these co-exposure patterns. A pilot study involving 20 healthy volunteers was conducted, with participants consuming either exclusively organic or conventional foods during a 24-h diet intervention in autumn 2021 and spring 2022 to account for seasonal variability. Participants provided detailed 24-h dietary records, and their first-morning urine samples were collected, minimally treated and analysed using LC-Q-ToF-MS by means of a multitargeted method in order to detect the presence of these residues. Results indicated that among the 52 screened compounds, four mycotoxins and seven pesticides were detected in over 25% of the samples. Deoxynivalenol (DON) and the non-specific pesticide metabolite diethylphosphate (DEP) exhibited the highest frequency rates (100%) and concentration levels. Correlations were observed between urine levels of mycotoxins (DON, ochratoxin alpha [OTα], and enniatin B [ENNB]) and organophosphate pesticide metabolites DEP and 2-diethylamino-6-methyl-4-pyrimidinol (DEAMPY). The pilot intervention study suggested a reduction in ENNB and OTα levels and an increase in β-zearalenol levels in urine after a short-term replacement with organic food. However, caution is advised due to the study's small sample size and short duration, emphasizing the need for further research to enhance understanding of the human chemical exposome and refine chemical risk assessment., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)
- Published
- 2024
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10. Tracing the dissipation of difenoconazole, its metabolites and co-formulants in tomato: A comprehensive analysis by chromatography coupled to high resolution mass spectrometry in laboratory and greenhouse trials.
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Maldonado-Reina AJ, López-Ruiz R, Marín Sáez J, Romero-González R, and Garrido Frenich A
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- Chromatography, High Pressure Liquid, Mass Spectrometry methods, Food Contamination analysis, Pesticide Residues analysis, Pesticide Residues metabolism, Solanum lycopersicum metabolism, Solanum lycopersicum chemistry, Dioxolanes metabolism, Triazoles metabolism, Triazoles analysis, Triazoles chemistry, Fungicides, Industrial metabolism, Fungicides, Industrial analysis
- Abstract
The study evaluated Ceremonia 25 EC®, a plant protection product (PPP) containing difenoconazole, in tomato crops, to identify potential risks associated with PPPs, and in addition to this compound, known metabolites from difenoconazole degradation and co-formulants present in the PPP were monitored. An ultra high performance liquid chromatography coupled to quadrupole-Orbitrap mass analyser (UHPLC-Q-Orbitrap-MS) method was validated with a working range of 2 μg/kg (limit of quantification, LOQ) to 200 μg/kg. Difenoconazole degradation followed a biphasic double first-order in parallel (DFOP) kinetic model in laboratory and greenhouse trials, with high accuracy (R
2 > 0.9965). CGA-205374, difenoconazole-alcohol, and hydroxy-difenoconazole metabolites were tentatively identified and semi-quantified in laboratory trials by UHPLC-Q-Orbitrap-MS from day 2 to day 30. No metabolites were found in greenhouse trials. Additionally, 13 volatile co-formulants were tentatively identified by gas chromatography (GC) coupled to Q-Orbitrap-MS, detectable up to the 7th day after PPP application. This study provides a comprehensive understanding of difenoconazole dissipation in tomatoes, identification of metabolites, and detection of co-formulants associated with the applied PPP., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 The Authors. Published by Elsevier Ltd.. All rights reserved.)- Published
- 2024
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11. Assessing human exposure to pesticides and mycotoxins: optimization and validation of a method for multianalyte determination in urine samples.
- Author
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Marín-Sáez J, Hernández-Mesa M, Gallardo-Ramos JA, Gámiz-Gracia L, and García-Campaña AM
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- Humans, Tandem Mass Spectrometry methods, Chromatography, Liquid methods, Chromatography, High Pressure Liquid methods, Mycotoxins analysis, Pesticides analysis, Pyrethrins analysis
- Abstract
Humans are exposed to an increasing number of contaminants, with diet being one of the most important exposure routes. In this framework, human biomonitoring is considered the gold standard for evaluating human exposure to chemicals. Pesticides and mycotoxins are chemicals of special concern due to their health implications. They constitute the predominant border rejection notifications for food and feed in Europe and the USA. However, current biomonitoring studies are focused on a limited number of compounds and do not evaluate mycotoxins and pesticides together. In this study, an analytical method has been developed for the determination of 30 pesticides and 23 mycotoxins of concern in urine samples. A salting-out liquid-liquid extraction (SALLE) procedure was optimized achieving recoveries between 70 and 120% for almost all the compounds and limits as lower as when QuEChERS was applied. The compounds were then determined by liquid chromatography coupled to triple quadrupole mass spectrometry. Different chromatographic conditions and analytical columns were tested, selecting a Hypersild gold aQ column as the best option. Finally, the method was applied to the analysis of 45 urine samples, in which organophosphate and pyrethroid pesticides (detection rates (DR) of 82% and 42%, respectively) and ochratoxin A and deoxynivalenol (DR of 51% and 33%, respectively) were the most detected compounds. The proposed analytical method involves the simultaneous determination of a diverse set of pesticides and mycotoxins, including their most relevant metabolites, in human urine. It serves as an essential tool for biomonitoring the presence of highly prevalent contaminants in modern society., (© 2024. The Author(s).)
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- 2024
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12. Holographic Sensor Based on Bayfol HX200 Commercial Photopolymer for Ethanol and Acetic Acid Detection.
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Potărniche IA, Marín-Sáez J, Collados MV, and Atencia J
- Abstract
This paper presents a holographic sensor based on reflection holograms recorded in the commercial photopolymer Bayfol
® HX 200. The recording geometry and index modulation of the hologram were optimised to improve accuracy for this specific application. The sensor was subjected to tests using various analytes, and it exhibited sensitivity to acetic acid and ethanol. The measurements revealed a correlation between the concentration of the analyte in contact with the sensor's surface and the resulting wavelength shift of the diffracted light. The minimum detectable concentrations were determined to be above 0.09 mol/dm3 for acetic acid and 5% ( v / v ) for ethanol. Notably, the sensors demonstrated a rapid response time. Given that ethanol serves as a base for alcoholic beverages, and acetic acid is commonly found in commercial vinegar, these sensors hold promise for applications in food quality control.- Published
- 2023
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13. Monitoring of Volatile Additives from Plant Protection Products in Tomatoes Using HS-SPME-GC-HRMS: Targeted and Suspect Approaches.
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Marín-Sáez J, López-Ruiz R, Romero-Gonzalez R, and Garrido Frenich A
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- Solid Phase Microextraction methods, Gas Chromatography-Mass Spectrometry methods, Toluene analysis, Solanum lycopersicum, Hydrocarbons, Aromatic, Volatile Organic Compounds analysis
- Abstract
Additives present in plant protection products (PPPs) are normally not monitored after sample treatments. In this study, the fate of additives detected by targeted and nontargeted analysis in tomato samples treated with two PPPs was carried out. The study was carried out in a greenhouse for 12 days, in which two applications with each PPP were made. Compounds were extracted by applying a headspace solid phase microextraction (HS-SPME) and analyzed by gas chromatography coupled to high resolution mass spectrometry (GC-HRMS), performing targeted and suspect approaches. Three targeted and 15 nontargeted compounds were identified at concentration levels of up to 150 μg/kg. Compounds detected encompassed benzene, toluene, indene, and naphthalene derivatives, as well as conservatives and flavouring compounds. Most of them degraded in less than 7 days after the second application, following first-order kinetic. This study aims to reduce knowledge gaps regarding additives and their fate under real climatic conditions of greenhouses cultivations.
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- 2023
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14. Gastrointestinal bioaccessibility and fiber mitigation of tropane alkaloids assessed on tea and cookies by in vitro digestion.
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Marín-Sáez J, Lopez-Ruiz R, Ferreira IMPLVO, and Cunha SC
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- Pectins, Gastrointestinal Tract, Tea chemistry, Digestion, Tropanes chemistry, Dietary Fiber
- Abstract
Background: Tropane alkaloids (TAs) are toxic compounds with a high anticholinergic effect. They have been widely analyzed in food samples, but their fate in the gastrointestinal tract has not been evaluated yet., Results: In this study, static in vitro digestion was performed to assess gastrointestinal bioaccessibility of the most common TAs on tea and home-made cookies. Cookies enriched with dietary fiber (pectin, arabinogalactan, and κ-carrageenan) were also tested to evaluate their influence on TA bioaccessibility. Two extraction methods and a liquid chromatography-mass spectrometry method were optimized and validated. Bioaccessibility for tea (60-105%) was higher than for cookies (39-93%) (P = 0.001-0.002), which indicates TAs could be more easily absorbed when they are contaminating tea. Digestion of cookies enriched with 50 g kg
-1 of different fibers showed that, although no significant changes were observed in the gastric phase (P = 0.084-0.920), duodenal bioaccessibility was significantly reduced (P = 0.008-0.039). Pectin was the fiber with a better mitigation effect for all the compounds., Conclusion: TAs bioaccessibility was determined after in vitro digestion of contaminated tea and cookies. Dietary fiber seems to be a promising mitigation strategy, significantly reducing TA bioaccessibility percentages. © 2023 The Authors. Journal of The Science of Food and Agriculture published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry., (© 2023 The Authors. Journal of The Science of Food and Agriculture published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry.)- Published
- 2023
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15. Uncovering the Dissipation of Chlorantraniliprole in Tomatoes: Identifying Transformation Products (TPs) and Coformulants in Greenhouse and Laboratory Studies by UHPLC-Q-Orbitrap-MS and GC-Q-Orbitrap-MS.
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Maldonado-Reina AJ, López-Ruiz R, Marín Sáez J, Romero-González R, Marín-Membrive P, and Garrido-Frenich A
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- Gas Chromatography-Mass Spectrometry, Chromatography, High Pressure Liquid methods, Mass Spectrometry methods, Solanum lycopersicum
- Abstract
The present study addressed the dissipation of the insecticide chlorantraniliprole in tomatoes treated with Altacor 35 WG under laboratory and greenhouse conditions, as well as the identification of transformation products (TPs) and coformulants, performing suspect screening analysis. Analyses were performed by ultra-high-performance liquid and gas chromatography coupled to quadrupole-Orbitrap high-resolution mass spectrometry (UHPLC-Q-Orbitrap-MS and GC-Q-Orbitrap-MS). In all cases, chlorantraniliprole was fitted to a biphasic kinetic model, with R
2 values greater than 0.99. Dissipation was noticeably faster in greenhouse studies, in which even 96% dissipation was achieved over 53 days. One TP, IN-F6L99, was tentatively identified in both greenhouse and laboratory studies and was semiquantified by using chlorantraniliprole as the analytical standard, yielding a top value of 354 μg/kg for laboratory studies, whereas values for greenhouse studies fell under the limit of quantitation (LOQ). Finally, a total of 15 volatile coformulants were identified by GC-Q-Orbitrap-MS.- Published
- 2023
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16. Comprehensive Dissipation of Azadirachtin in Grapes and Tomatoes: The Effect of Bacillus thuringiensis and Tentative Identification of Unknown Metabolites.
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Marín-Sáez J, López-Ruiz R, Romero-Gonzalez R, and Garrido Frenich A
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- Bacillus thuringiensis, Solanum lycopersicum, Vitis
- Abstract
Neem oil is a biopesticide normally applied together with Bacillus thuringiensis ( Bt ) . However, neither its dissipation nor the influence of Bt has been previously evaluated. In this study, dissipation of neem oil was investigated when it was applied alone or together with Bt at 3 and 22 °C. A methodology involving solid-liquid extraction and liquid chromatography-high-resolution mass spectrometry was developed for that purpose. The method was validated obtaining recoveries from 87 to 103%, with relative standard deviations lower than 19% and limits of quantification from 5 to 10 μg/kg. Azadirachtin A (AzA) dissipation was fit to a single first order, being faster when neem oil was applied together with Bt and at 22 °C (RL
50 = 12-21 days) than alone and at 3 °C (RL50 = 14-25 days). Eight related compounds were found in real samples with similar dissipation curves compared to AzA, and five unknown metabolites were identified in degraded samples, with increasing concentrations during parent compound degradation.- Published
- 2023
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17. Critical Evaluation of Analytical Methods for the Determination of Anthropogenic Organic Contaminants in Edible Oils: An Overview of the Last Five Years.
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López-Ruiz R, Marín-Sáez J, Prestes OD, Romero-González R, and Garrido Frenich A
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- Oils chemistry, Gas Chromatography-Mass Spectrometry methods, Chromatography, High Pressure Liquid, Polycyclic Aromatic Hydrocarbons analysis, Pesticides analysis
- Abstract
Anthropogenic contaminants, as pesticides, polycyclic aromatic hydrocarbons (PAHs) and monochloropropanediols (MCPDs), have become important to be controlled in edible oils, since their regular occurrence. In fact, alerts from the Rapid Alert System for Food and Feed (RASFF) in oils normally include these compounds. From a critical point of view, tools used to control these compounds in the last 5 years will be discussed, including sample preparation, analysis and current regulations. Extraction and analysis methods will be discussed next, being liquid-liquid extraction (LLE) and QuEChERS, with or without clean-up step, as well as chromatographic methods coupled to different analyzers (mainly mass spectrometry), the most commonly used for extraction and analysis respectively. Occurrence in samples will also be reviewed and compared with the legal maximum residue limits (MRLs), observing that 4%, 20% and 60% of the analyzed samples exceed the legal limits for pesticides, MCPDs and PAHs respectively.
- Published
- 2023
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18. Looking beyond the Active Substance: Comprehensive Dissipation Study of Myclobutanil-Based Plant Protection Products in Tomatoes and Grapes Using Chromatographic Techniques Coupled to High-Resolution Mass Spectrometry.
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Marín-Sáez J, López-Ruiz R, Romero-Gonzalez R, Garrido Frenich A, and Zamora Rico I
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- Chromatography, High Pressure Liquid methods, Gas Chromatography-Mass Spectrometry, Mass Spectrometry, Nitriles, Triazoles, Solanum lycopersicum chemistry, Vitis
- Abstract
A comprehensive evaluation of the dissipation of a myclobutanil plant protection product was performed in tomato and grape samples. Different temperature conditions (3 and 22 °C) were evaluated. A biphasic kinetic model provided a suitable adjustment ( R
2 > 0.95), with persistence (residual level, RL50 ) lower than 24 days in all cases. Solid-liquid extraction and ultra-high-performance liquid chromatography coupled to high-resolution mass spectrometry (UHPLC-Q-Orbitrap-HRMS) were used for metabolites' elucidation, identifying six myclobutanil metabolites, four out of them described for the first time and one of them confirmed using1 H,13 C, (1 H-1 H)-COSY, (1 H-13 C)-HMQC, and (1 H-13 C)-HMBC nuclear magnetic resonance (NMR). Their degradation curves were also evaluated, increasing their concentrations when the myclobutanil concentration decreases. Additionally, coformulants present in the commercial formulation were monitored employing headspace solid-phase microextraction method (HS-SPME)-gas chromatography coupled to HRMS (GC-Q-Orbitrap-HRMS). Seven coformulants were quantified in tomato samples. Their dissipation curves were studied, and it was observed that they were almost degraded 12 days after application.- Published
- 2022
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19. Recent applications of chromatography for analysis of contaminants in cannabis products: a review.
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López-Ruiz R, Marín-Sáez J, Garrido Frenich A, and Romero-González R
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- Chromatography, Liquid, Gas Chromatography-Mass Spectrometry, Mass Spectrometry, Cannabis, Pesticides analysis
- Abstract
In the last few years, the cultivation of cannabis has been increasing due to greater use in foods, recreational use, creams, oils, and other applications. Thus, analysis of contaminants (e.g. pesticides and mycotoxins) in cannabis products is necessary to ensure consumer safety. This review is focused on the analytical procedures, based on chromatographic techniques, used for the determination of contaminants in cannabis and related products, developed from 2015 to 2020. QuEChERS (acronym of quick, easy, cheap, effective, rugged and safe) was mainly used for the extraction of pesticides and other contaminants from cannabis because its versatility and capacity to extract a wide range of substances, and therefore, increasing the scope of the analysis. The most employed technique to determine pesticides and mycotoxins in cannabis products was liquid chromatography (LC) coupled to mass spectrometry (MS), although gas chromatography (GC) coupled to MS was also employed for the analysis of non-polar compounds, using triple quadrupole (QqQ) as mass analyzer. Nevertheless, new advances in cannabis analysis are also discussed, introducing techniques such as high-resolution mass spectrometry (HRMS), which allows for performing both targeted and untargeted (unknown and suspect) analyses. © 2021 Society of Chemical Industry., (© 2021 Society of Chemical Industry.)
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- 2022
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20. In Vivo Characterization of the Toxicological Properties of DPhP, One of the Main Degradation Products of Aryl Phosphate Esters.
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Selmi-Ruby S, Marín-Sáez J, Fildier A, Buleté A, Abdallah M, Garcia J, Deverchère J, Spinner L, Giroud B, Ibanez S, Granjon T, Bardel C, Puisieux A, Fervers B, Vulliet E, Payen L, and Vigneron AM
- Subjects
- Animals, Esters toxicity, Mice, Models, Chemical, Toxicity Tests, Environmental Pollutants toxicity, Phosphates toxicity
- Abstract
Background: Aryl phosphate esters (APEs) are widely used and commonly present in the environment. Health hazards associated with these compounds remain largely unknown and the effects of diphenyl phosphate (DPhP), one of their most frequent derivatives, are poorly characterized., Objective: Our aim was to investigate whether DPhP per se may represent a more relevant marker of exposure to APEs than direct assessment of their concentration and determine its potential deleterious biological effects in chronically exposed mice., Methods: Conventional animals (FVB mice) were acutely or chronically exposed to relevant doses of DPhP or to triphenyl phosphate (TPhP), one of its main precursors. Both molecules were measured in blood and other tissues by liquid chromatography-mass spectrometry (LC-MS). Effects of chronic DPhP exposure were addressed through liver multi-omics analysis to determine the corresponding metabolic profile. Deep statistical exploration was performed to extract correlated information, guiding further physiological analyses., Results: Multi-omics analysis confirmed the existence of biological effects of DPhP, even at a very low dose of 0.1 mg / mL in drinking water. Chemical structural homology and pathway mapping demonstrated a clear reduction of the fatty acid catabolic processes centered on acylcarnitine and mitochondrial β -oxidation in mice exposed to DPhP in comparison with those treated with vehicle. An interesting finding was that in mice exposed to DPhP, mRNA, expression of genes involved in lipid catabolic processes and regulated by peroxisome proliferator-activated receptor alpha ( PPAR α ) was lower than that in vehicle-treated mice. Immunohistochemistry analysis showed a specific down-regulation of HMGCS2, a kernel target gene of PPAR α . Overall, DPhP absorption disrupted body weight-gain processes., Conclusions: Our results suggest that in mice, the effects of chronic exposure to DPhP, even at a low dose, are not negligible. Fatty acid metabolism in the liver is essential for controlling fast and feast periods, with adverse consequences on the overall physiology. Therefore, the impact of DPhP on circulating fat, cardiovascular pathologies and metabolic disease incidence deserves, in light of our results, further investigations. https://doi.org/10.1289/EHP6826.
- Published
- 2020
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21. Degradation of tropane alkaloids in baked bread samples contaminated with Solanaceae seeds.
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Marín-Sáez J, Romero-González R, and Garrido Frenich A
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- Chromatography, Liquid, Datura stramonium chemistry, Fagopyrum chemistry, Fermentation, Food Analysis, Food Contamination analysis, Food Handling, Tropanes analysis, Alkaloids analysis, Bread analysis, Seeds chemistry, Solanaceae chemistry, Tropanes chemistry
- Abstract
Solanaceae plant seeds, which contain high concentrations of tropane alkaloids, have not been studied in real conditions of proofing and baking processes. In this work both lab vial trials and buckwheat and millet flour samples, contaminated with two species of Solanaceae plants, Datura stramonium and Brugmansia arborea, were undergone to proofing (37 °C) and baking (190 °C) processes. For the determination of tropane alkaloids, a simple solid-liquid extraction with methanol:water 2:1 (v/v) containing 0.5% acetic acid was used to extract the targeted compounds, whereas a chromatographic method employing a Zorbax C
18 column coupled to an Exactive-Orbitrap analyser was used for their determination. The results indicate that concentrations of tropane alkaloids decrease under proofing conditions (degradation between 13 and 95%), while they are almost disappeared under baking conditions (degradation between 94 and 100%). Some degradation pathways have been clarified, showing that most of the compounds degrade into tropane and tropine, and into tropine and tropinone under proofing and baking conditions respectively., (Copyright © 2019 Elsevier Ltd. All rights reserved.)- Published
- 2019
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22. Effect of tea making and boiling processes on the degradation of tropane alkaloids in tea and pasta samples contaminated with Solanaceae seeds and coca leaf.
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Marín-Sáez J, Romero-González R, and Garrido Frenich A
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- Acetone analogs & derivatives, Acetone chemistry, Chromatography, Liquid, Datura stramonium, Fagopyrum, Mass Spectrometry, Plant Leaves, Pyrrolidines chemistry, Seeds, Solid Phase Extraction, Transition Temperature, Coca, Food Contamination, Solanaceae, Tea chemistry, Tropanes chemistry
- Abstract
In this study, the degradation of tropane alkaloids in pasta under boiling (100 °C during 10 min) and tea making (100 °C and let cool 5 min) conditions has been evaluated for the first time. Pasta and green tea were contaminated with Datura Stramonium and Brugmansia Arborea seeds (pasta and green tea), whereas coca leaf tea was directly analysed. The compounds were extracted using solid-liquid extraction coupled to a preconcentration stage (only for the cooking water), and the compounds were analysed by liquid chromatography coupled to mass spectrometry (Exactive-Orbitrap analyser). Degradation studies indicate that concentration of tropane alkaloids decreases, and it depends on the compound, observing the highest degradation for tropinone, tropane, cuscohygrine and tropine, as well as it was observed that compounds migrated to the aqueous phase during cooking step. Finally, post-targeted analysis was performed and other tropane alkaloids were found, as scopine, tigloidine or convolvine, showing a similar behaviour under cooking conditions., (Copyright © 2019 Elsevier Ltd. All rights reserved.)
- Published
- 2019
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23. Reliable determination of tropane alkaloids in cereal based baby foods coupling on-line spe to mass spectrometry avoiding chromatographic step.
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Marín-Sáez J, Romero-González R, and Garrido Frenich A
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- Alkaloids isolation & purification, Atropine analysis, Humans, Infant, Scopolamine analysis, Solid Phase Extraction, Tandem Mass Spectrometry, Alkaloids analysis, Infant Food analysis, Spectrometry, Mass, Electrospray Ionization, Tropanes chemistry
- Abstract
Cereal based foods are a major part of the infant diet and they can be contaminated with Solanaceae and other plants containing tropane alkaloids. This study was focused on the optimisation of an extraction procedure based on a solid-liquid method and an online SPE system, directly coupled to different mass spectrometry analysers as Orbitrap and triple quadrupole (QqQ), removing the chromatographic separation step. Total running analysis time was 15.8 min (17.3 min in the QqQ system). The developed method was validated obtaining recoveries ranging from 66 to 98% and 68-97% for the Orbitrap and QqQ respectively (RSD lower than 14.3%) and limits of quantification from 0.5 to 5 µg kg
-1 and 0.5-10 µg kg-1 for the QqQ and Orbitrap analyser respectively. The validated method was applied to several cereal based baby food samples, finding a positive sample containing atropine (11.5 µg kg-1 ), scopolamine (2.8 µg kg-1 ) and apoatropine (7.5 µg kg-1 )., (Copyright © 2018 Elsevier Ltd. All rights reserved.)- Published
- 2019
- Full Text
- View/download PDF
24. Optimization and establishment of QuEChERS based method for determination of propoxycarbazone and its metabolite in food commodities by liquid chromatography coupled to tandem mass spectrometry.
- Author
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Vargas-Pérez M, Marín-Sáez J, Egea González FJ, and Garrido Frenich A
- Subjects
- Calibration, Chromatography, High Pressure Liquid, Food Contamination analysis, Linear Models, Benzoates analysis, Benzoates metabolism, Costs and Cost Analysis, Food Analysis economics, Food Analysis methods, Safety, Tandem Mass Spectrometry, Triazoles analysis, Triazoles metabolism
- Abstract
This study reports a method for propoxycarbazone pesticide determination including its metabolite in food commodities (lettuce, beetroot, soybean meal and honey). Both compounds were extracted, and samples cleaned using a buffered QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method based on the AOAC Official Method, followed by ultra high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). Both matrix-matched calibration curves showed good linearity (R
2 = 0.99) within the tested ranges. Method performance was assessed on the basis of recovery and intra/inter-day precision studies at spiked concentrations of 10 (25) and 50 µg/kg (n = 5). Mean recovery rates were between 73 and 110%, while precision studies, assessed by relative standard deviation (RSD), were ≤20%. The limits of quantification (LOQ) were established as 10 or 25 µg/kg, depending on the matrix, which are low enough for monitoring residues at regulated maximum residue levels., (Copyright © 2018 Elsevier Ltd. All rights reserved.)- Published
- 2019
- Full Text
- View/download PDF
25. Screening of drugs and homeopathic products from Atropa belladonna seed extracts: Tropane alkaloids determination and untargeted analysis.
- Author
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Marín-Sáez J, Romero-González R, Garrido Frenich A, and Egea-González FJ
- Subjects
- Atropine analysis, Chromatography, High Pressure Liquid methods, Scopolamine analysis, Tandem Mass Spectrometry methods, Alkaloids analysis, Atropa belladonna chemistry, Plant Extracts chemistry, Seeds chemistry, Tropanes analysis
- Abstract
Homeopathic products are still a controversial issue in modern medicine, understood as complementary or alternative medicine (CAM). In this particular case, homeopathic products prepared from Atropa belladonna extracts may present specific problems due to the effects derived from its components. This article applies a simple, rapid, reliable method to the analysis of different homeopathic products obtained from Atropa belladonna; drugs containing high concentration of plant extracts; and Atropa belladonna seeds. The method was based on a simple solid-phase preconcentration method followed by ultra-high pressure liquid chromatography (UHPLC) coupled to high resolution mass spectrometry using Exactive-Orbitrap as an analyser. An in-house database was set and atropine and scopolamine were the compounds detected at highest concentrations in homeopathic products from Atropa belladonna extracts (4.57 and 2.56 μg/kg, respectively), in Belladonna ointment (4007 and 1139 μg/kg, respectively) and Belladonna seeds (338 and 32.1 mg/kg, respectively). Other tropane alkaloids such as tropine, apoatropine, aposcopolamine, tropinone, homatropine, and anisodamine were detected at lower concentrations (0.04-1.36 μg/kg). When untargeted analysis was performed, other tropane alkaloids were identified in the tested samples, such as ecgonine (0.003 μg/kg), benzoylecgonine (0.56 μg/kg), calystegines A (19.6 μg/kg), B (33.1 μg/kg), and C (1.01 μg/kg). Finally other compounds present in the homeopathic products, such as sugars (fructose, glucose, and lactose) or amino acids (valine, ornithine, leucine, and phenylalanine), were identified., (Copyright © 2018 John Wiley & Sons, Ltd.)
- Published
- 2018
- Full Text
- View/download PDF
26. Full modeling and experimental validation of cylindrical holographic lenses recorded in Bayfol HX photopolymer and partly operating in the transition regime for solar concentration.
- Author
-
Marín-Sáez J, Atencia J, Chemisana D, and Collados MV
- Abstract
Concentrating photovoltaics for building integration can be successfully carried out with Holographic Optical Elements (HOEs) because of their behavior analogous to refractive optical elements and their tuning ability to the spectral range that the photovoltaic (PV) cell is sensitive to. That way, concentration of spectral ranges that would cause overheating of the cell is avoided. Volume HOEs are usually chosen because they provide high efficiencies. However, their chromatic selectivity is also very high, and only a small part of the desired spectral range reaches the PV cell. A novel approach is theoretically and experimentally explored to overcome this problem: the use of HOEs operating in the transition regime, which yield lower chromatic selectivity while keeping rather high efficiencies. A model that considers the recording material's response, by determining the index modulation reached for each spatial frequency and exposure dosage, has been developed. It has been validated with experimental measurements of three cylindrical holographic lenses with different spatial frequency ranges recorded in Bayfol HX photopolymer. Simulations of systems comprising two lenses and a mono-c Si PV cell are carried out with the standard AM 1.5D solar spectrum. Promising results are obtained when using the system with lower spatial frequencies lenses: a total current intensity equal to 3.72 times the one that would be reached without the concentrator.
- Published
- 2018
- Full Text
- View/download PDF
27. Multi-analysis determination of tropane alkaloids in cereals and solanaceaes seeds by liquid chromatography coupled to single stage Exactive-Orbitrap.
- Author
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Marín-Sáez J, Romero-González R, and Garrido Frenich A
- Subjects
- Chromatography, Liquid, Limit of Detection, Tropanes chemistry, Alkaloids analysis, Edible Grain chemistry, Food Contamination analysis, Food Technology methods, Seeds chemistry, Solanaceae chemistry, Tropanes analysis
- Abstract
Tropane alkaloids are a wide group of substances that comprises more than 200 compounds occurring especially in the Solanaceae family. The main aim of this study is the development of a method for the analysis of the principal tropane alkaloids as atropine, scopolamine, anisodamine, tropane, tropine, littorine, homatropine, apoatropine, aposcopolamine, scopoline, tropinone, physoperuvine, pseudotropine and cuscohygrine in cereals and related matrices. For that, a simple solid-liquid extraction was optimized and a liquid chromatographic method coupled to a single stage Exactive-Orbitrap was developed. The method was validated obtaining recoveries in the range of 60-109% (except for some compounds in soy), precision values (expressed as relative standard deviation) lower than 20% and detection and quantification limits equal to or lower than 2 and 3μg/kg respectively. Finally, the method was applied to the analysis of different types of samples as buckwheat, linseed, soy and millet, obtaining positives for anisodamine, scopolamine, atropine, littorine and tropinone in a millet flour sample above the quantification limits, whereas atropine and scopolamine were detected in a buckwheat sample, below the quantification limit. Contaminated samples with Solanaceaes seeds (Datura Stramonium and Brugmansia Arborea) were also analysed, detecting concentrations up to 693μg/kg (scopolamine) for contaminated samples with Brugmansia seeds and 1847μg/kg (atropine) when samples were contaminated with Stramonium seeds., (Copyright © 2017 Elsevier B.V. All rights reserved.)
- Published
- 2017
- Full Text
- View/download PDF
28. Simultaneous determination of atropine and scopolamine in buckwheat and related products using modified QuEChERS and liquid chromatography tandem mass spectrometry.
- Author
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Chen H, Marín-Sáez J, Romero-González R, and Garrido Frenich A
- Subjects
- Atropine isolation & purification, Fagopyrum growth & development, Scopolamine isolation & purification, Water chemistry, Atropine analysis, Chromatography, Liquid methods, Fagopyrum metabolism, Scopolamine analysis, Solid Phase Extraction methods, Tandem Mass Spectrometry methods
- Abstract
A method was developed for the determination of atropine and scopolamine in buckwheat and related products. A modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) extraction procedure was evaluated. Dispersive solid phase extraction (d-SPE) was studied as clean-up step, using graphitized black carbon (GBC) and primary secondary amine (PSA). The extract was diluted with water (50:50, v/v) prior to chromatographic analysis. The method was validated and recoveries (except chia samples spiked at 10μg/kg) ranged from 75% to 92%. Intra and inter-day precision was lower than or equal to 17%. The limit of quantification of atropine and scopolamine was 0.4 and 2μg/kg, respectively. Eight types of samples (buckwheat, wheat, soy, buckwheat flour, buckwheat noodle, amaranth grain, chia seeds and peeled millet) were analyzed. Target compounds were not found above the detection limits of the method, but three transformation products of scopolamine (norscopine, hydroscopolamine and dihydroxyscopolamine) were putative identified in the tested samples using high resolution mass spectrometry (Exactive-Orbitrap)., (Copyright © 2016 Elsevier Ltd. All rights reserved.)
- Published
- 2017
- Full Text
- View/download PDF
29. Enantiomeric determination and evaluation of the racemization process of atropine in Solanaceae seeds and contaminated samples by high performance liquid chromatography-tandem mass spectrometry.
- Author
-
Marín-Sáez J, Romero-González R, and Garrido Frenich A
- Subjects
- Atropine isolation & purification, Chromatography, High Pressure Liquid, Datura stramonium chemistry, Fagopyrum chemistry, Hydrogen-Ion Concentration, Hyoscyamine analysis, Indicators and Reagents, Limit of Detection, Reproducibility of Results, Seeds chemistry, Solvents, Stereoisomerism, Tandem Mass Spectrometry, Temperature, Atropine chemistry, Solanaceae chemistry
- Abstract
A new method has been developed for the enantioselective separation of (-) and (+) hyoscyamine in Solanaceaes seeds and contaminated buckwheat. Chromatographic separation was optimized, evaluating two chiral columns, Chirobiotic V and Chiralpal-AY3. Better resolution was obtained using a Chiralpak-AY3 column, utilizing as mobile phase ethanol (0.1% diethanolamine). An extraction procedure based on a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) was applied, using water and acetonitrile containing 1% of acetic acid, and a clean-up step utilizing primary secondary amine (PSA) and graphitized carbon black (GCB) as sorbents. The extract was diluted with ethanol (50/:50, v/v) prior to chromatographic analysis, and the separation was carried out avoiding the racemization during this stage. Enantiomerization process of atropine was studied in samples at different conditions such as temperature (30, 50 and 80°C) and pH (3, 5, 7 and 9), observing that racemization occurs at high pH (9) and temperature (80°C). Stramonium and Brugmansia seeds were analyzed and the concentration of (-)-hyoscyamine was 1500mg/kg and 320mg/kg respectively. Contaminated buckwheat was also determined and (-)-hyoscyamine was detected at 170μg/kg., (Copyright © 2016 Elsevier B.V. All rights reserved.)
- Published
- 2016
- Full Text
- View/download PDF
30. Characterization of volume holographic optical elements recorded in Bayfol HX photopolymer for solar photovoltaic applications.
- Author
-
Marín-Sáez J, Atencia J, Chemisana D, and Collados MV
- Abstract
Volume Holographic Optical Elements (HOEs) present interesting characteristics for photovoltaic applications as they can select spectrum for concentrating the target bandwidth and avoiding non-desired wavelengths, which can cause the decrease of the performance on the cell, for instance by overheating it. Volume HOEs have been recorded on Bayfol HX photopolymer to test the suitability of this material for solar concentrating photovoltaic systems. The HOEs were recorded at 532 nm and provided a dynamic range, reaching close to 100% efficiency at 800 nm. The diffracted spectrum had a FWHM of 230 nm when illuminating at Bragg angle. These characteristics prove HOEs recorded on Bayfol HX photopolymer are suitable for concentrating solar light onto photovoltaic cells sensitive to that wavelength range.
- Published
- 2016
- Full Text
- View/download PDF
31. Broadband behavior of transmission volume holographic optical elements for solar concentration.
- Author
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Bañares-Palacios P, Álvarez-Álvarez S, Marín-Sáez J, Collados MV, Chemisana D, and Atencia J
- Abstract
A ray tracing algorithm is developed to analyze the energy performance of transmission and phase volume holographic lenses that operate with broadband illumination. The agreement between the experimental data and the theoretical treatment has been tested. The model has been applied to analyze the optimum recording geometry for solar concentration applications.
- Published
- 2015
- Full Text
- View/download PDF
32. Holographic optical element to generate achromatic vortices.
- Author
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Atencia J, Collados MV, Quintanilla M, Marín-Sáez J, and Sola IJ
- Abstract
A compound holographic optical element to generate achromatic vortices with high efficiency, based on the combination of two volume phase holograms, is designed and constructed. This element is compact and easy to align. It has high damage threshold, so it can be used with ultraintense laser pulses.
- Published
- 2013
- Full Text
- View/download PDF
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