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1.
Environ Monit Assess ; 196(11): 1015, 2024 Oct 04.
Article in English | MEDLINE | ID: mdl-39365363

ABSTRACT

The study was conducted in Cerritos, San Luis Potosí, México, near the Guaxcama mine, focused on environmental contamination (groundwater and agricultural soil) from antimony (Sb), arsenic (As), lead (Pb), cadmium (Cd), and mercury (Hg). In March 2022, 20 agricultural soil and 16 groundwater samples were collected near the historically cinnabar (HgS)- and arsenopyrite (FeAsS)-rich Guaxcama mine. Hydride generation atomic fluorescence spectrometry (HG-AFS) for As, cold vapor atomic fluorescence spectrometry (CV-AFS) for Hg, and inductively coupled plasma optical emission spectrometry (ICP-OES) for Cd, Pb, and Sb were used for the determinations of potentially toxic elements (PTEs). While concentrations of Cd, Hg, Pb, and Sb in groundwater were below detection limits, As levels exhibited a range from 40.9 ± 1.4 to 576.0 ± 1.0 µg/L, exceeding permissible limits for drinking water (10 µg/L). In agricultural soil, As was between 7.67 ± 0.16 and 24.1 ± 0.4 µg/g, Hg ranged from 0.203 ± 0.018 to 2.33 ± 0.19 µg/g, Cd from 2.53 ± 0.90 to 2.78 ± 0.01 µg/g, and Pb from 11.7 ± 1.2 to 34.3 ± 4.1 µg/g. Only one study area surpassed the Mexican As soil limit of 22 µg/g. Sequential extraction (four-step BCR procedure) indicated significant As bioavailability in soil (fractions 1 and 2) ranging from 3.66 to 10.36%, heightening the risk of crop transfer, in contrast to the low bioavailability of Hg, showing that fractions 1, 2, and 3 were below the limit of quantification (LOQ). Crucial physicochemical parameters in soil, including nitrate levels, pH, and organic matter, were pivotal in understanding contamination dynamics. Principal component analysis highlighted the influence of elements like Fe and Ca on phytoavailable As, while Pb and Cd likely originated from a common source. Ecological risk assessments underscored the significant impact of pollution, primarily due to the concentrations of Cd and Hg. Non-cancer and cancer risks to residents through As poisoning via contaminated water ingestion also were found. The hazard index (HI) values varied between 4.0 and 82.2 for adults and children. The total incremental lifetime cancer risk (TILCAR) values for adults ranged from 7.75E - 04 to 1.06E - 02, whereas for children, the values were from 2.47E - 04 to 3.17E - 03.


Subject(s)
Agriculture , Antimony , Arsenic , Environmental Monitoring , Groundwater , Mining , Soil Pollutants , Water Pollutants, Chemical , Mexico , Groundwater/chemistry , Soil Pollutants/analysis , Water Pollutants, Chemical/analysis , Arsenic/analysis , Antimony/analysis , Mercury/analysis , Cadmium/analysis , Soil/chemistry , Lead/analysis , Metals, Heavy/analysis
2.
Environ Res ; 258: 119477, 2024 Oct 01.
Article in English | MEDLINE | ID: mdl-38909943

ABSTRACT

In this study, UiO-67 (Zr)/g-C3N4 composites (U67N) were synthesized at wt.% ratios of 05:95, 15:85, and 30:70 using the solvothermal method at 80 °C for 24 h followed by calcination at 350 °C. The composites were characterized using UV-Vis diffuse reflectance spectroscopy, Fourier-transform infrared spectroscopy, photoluminescence spectroscopy, X-ray photoelectron spectroscopy, X-ray diffraction, scanning electron microscopy-energy-dispersive X-ray spectroscopy, transmission electron microscopy, and nitrogen physisorption analysis. In addition, thermal stability analysis of UiO-67 was conducted using thermogravimetric analysis. The photocatalytic performance of the composites was assessed during the degradation and mineralization of a mixture of methylparaben (MeP) and propylparaben (PrP) under simulated sunlight. The adsorption process of U67N 15:85 was characterized through kinetic studies and adsorption capacity experiments, which were modeled using pseudo-first-order and pseudo-second-order kinetics and Langmuir and Freundlich isotherms, respectively. The influence of pH levels 3, 5, and 7 on the photocatalytic degradation of the mixture was investigated, revealing enhanced degradation and mineralization at pH 3. The U67N composite exhibited dual capability in removing contaminants through adsorption and photocatalytic processes. Among the prepared composites, U67N 15:85 demonstrated the highest photocatalytic activity, achieving removal efficiencies of 96.8% for MeP, 92.5% for PrP, and 45.7% for total organic carbon in 300 kJ/m2 accumulated energy (3 h of reaction time). The detoxification of the effluent was confirmed through acute toxicity evaluation using the Vibrio fischeri method. The oxidation mechanism of the heterojunction formed between UiO-67 (Zr) and g-C3N4 was proposed based on PL analysis, photoelectrochemistry studies (including photocurrent response, Nyquist, and Mott-Schottky analyses), and scavenger assays.


Subject(s)
Parabens , Water Pollutants, Chemical , Parabens/chemistry , Adsorption , Water Pollutants, Chemical/chemistry , Metal-Organic Frameworks/chemistry , Catalysis , Kinetics
3.
Methods Mol Biol ; 2745: 45-75, 2024.
Article in English | MEDLINE | ID: mdl-38060179

ABSTRACT

The thermodynamic formalism of nonequilibrium systems together with the theory of complex systems and systems biology offer an appropriate theoretical framework to explain the complexity observed at the macroscopic level in physiological phenomena. In turn, they allow the establishment of an appropriate conceptual and operational framework to address the study of phenomena such as the emergence and evolution of cancer.This chapter is organized as follows: In Subheading 1, an integrated vision of these disciplines is offered for the characterization of the emergence and evolution of cancer, seen as a nonlinear dynamic system, temporally and spatially self-organized out of thermodynamic equilibrium. The development of the various mathematical models and different techniques and approaches used in the characterization of cancer metastasis is presented in Subheading 2. Subheading 3 is devoted to the time course of cancer metastasis, with particular emphasis on the epithelial-mesenchymal transition (EMT henceforth) as well as chronotherapeutic treatments. In Subheading 4, models of the spatial evolution of cancer metastasis are presented. Finally, in Subheading 5, some conclusions and remarks are presented.


Subject(s)
Models, Theoretical , Neoplasms , Humans , Thermodynamics , Neoplasms/pathology , Nonlinear Dynamics , Epithelial-Mesenchymal Transition
4.
Chemosphere ; 335: 139010, 2023 Sep.
Article in English | MEDLINE | ID: mdl-37236281

ABSTRACT

Heavy metals (HMs) and metalloids (Ms) such as arsenic (As), cadmium (Cd), mercury (Hg), and lead (Pb) represent serious environmental threats due to their wide abundance and high toxicity. Contamination of water and soils by HMs and Ms from natural or anthropogenic sources is of great concern in agricultural production due to their toxic effects on plants, adversely affecting food safety and plant growth. The uptake of HMs and Ms by Phaseolus vulgaris L. plants depends on several factors including soil properties such as pH, phosphate, and organic matter. High concentrations of HMs and Ms could be toxic to plants due to the increased generation of reactive oxygen species (ROS) such as (O2•-), (•OH), (H2O2), and (1O2), and oxidative stress due to an imbalance between ROS generation and antioxidant enzyme activity. To minimize the effects of ROS, plants have developed a complex defense mechanism based on the activity of antioxidant enzymes such as SOD, CAT, GPX, and phytohormones, especially salicylic acid (SA) that can reduce the toxicity of HMs and Ms. This review focuses on evaluating the accumulation and translocation of As, Cd, Hg, and Pb in Phaseolus vulgaris L. plants and on their possible effects on the growth of Phaseolus vulgaris L. in soil contaminated with these elements. The factors that affect the uptake of HMs and Ms by bean plants, and the defense mechanisms under oxidative stress caused by the presence of As, Cd, Hg, and Pb are also discussed. Furthermore, future research on mitigating HMs and Ms toxicity in Phaseolus vulgaris L. plants is highlighted.


Subject(s)
Arsenic , Mercury , Metalloids , Metals, Heavy , Phaseolus , Soil Pollutants , Cadmium/toxicity , Reactive Oxygen Species/pharmacology , Antioxidants/pharmacology , Hydrogen Peroxide/pharmacology , Lead/pharmacology , Soil Pollutants/analysis , Metals, Heavy/analysis , Arsenic/analysis , Mercury/toxicity , Plants , Soil/chemistry
5.
Neurologia (Engl Ed) ; 36(6): 418-425, 2021.
Article in English | MEDLINE | ID: mdl-34238524

ABSTRACT

INTRODUCTION: The handling of information through digital media allows innovative approaches for identifying cases of dementia through computerised searches within the clinical databases that include systems for coding diagnoses. The aim of this study was to analyse the validity of a dementia registry in Gipuzkoa based on the administrative and clinical databases existing in the Basque Health Service. METHODS: This is a descriptive study based on the evaluation of available data sources. First, through review of medical records, the diagnostic validity was evaluated in two samples of cases identified and not identified as dementia. The sensitivity, specificity and positive and negative predictive value of the diagnosis of dementia were measured. Subsequently, the cases of living dementia in December 31, 2016 were searched in the entire Gipuzkoa population to collect sociodemographic and clinical variables. RESULTS: The validation samples included 986 cases and 327 no cases. The calculated sensitivity was 80.2% and the specificity was 99.9%. The negative predictive value was 99.4% and positive value was 95.1%. The cases in Gipuzkoa were 10 551, representing 65% of the cases predicted according to the literature. Antipsychotic medication were taken by a 40% and a 25% of the cases were institutionalised. CONCLUSIONS: A registry of dementias based on clinical and administrative databases is valid and feasible. Its main contribution is to show the dimension of dementia in the health system.


Subject(s)
Dementia , Registries , Alzheimer Disease , Dementia/diagnosis , Humans , Internet , Spain
6.
Food Chem ; 232: 493-500, 2017 Oct 01.
Article in English | MEDLINE | ID: mdl-28490103

ABSTRACT

The development of a new method to determine the presence of the organoarsenic additives p-arsanilic acid (ASA), roxarsone (ROX) and nitarsone (NIT) in livestock feeds by high performance liquid chromatography coupled to ultraviolet oxidation hydride generation atomic fluorescence spectrometry (HPLC-UV/HG-AFS) after microwave assisted extraction (MAE) was proposed. Chromatographic separation was achieved on a C18 column with 2% acetic acid/methanol (96:4, v/v) as the mobile phase. The limits of detection (LODs) were 0.13, 0.09 and 0.08mgL-1, and the limits of quantification (LOQs) were 0.44, 0.30 and 0.28mgL-1. The relative standard deviations (RSDs) for ASA, ROX and NIT determined from five measurements of the mixed calibration standard were 3.3, 5.3, and 5.4%, respectively. MAE extraction of phenylated arsenic compounds using 1.5M H3PO4 at 120°C for 45min allowed for maximum recoveries (%) of total arsenic (As) and organoarsenic species, with no degradation of these compounds. The extraction of total As was approximately 97%, and the As species recoveries were between 95.2 and 97.0%. The results of the analysis were validated using mass balance by comparing the sum of extracted As with the total concentration of As in the corresponding samples. The method was successfully applied to determine the presence of these compounds in feed samples. ASA was the only As species detected in chicken feed samples, with a concentration between 0.72 and 12.91mgkg-1.


Subject(s)
Animal Feed , Livestock , Animals , Arsenic , Chromatography, High Pressure Liquid , Food Analysis , Microwaves , Spectrometry, Fluorescence
7.
Environ Sci Pollut Res Int ; 24(5): 4613-4624, 2017 Feb.
Article in English | MEDLINE | ID: mdl-27966080

ABSTRACT

In this study, the photocatalytic removal of an emerging contaminant, diclofenac (DCF) sodium, was performed using the nitrogen-doped WO3/TiO2-coupled oxide catalyst (WO3/TiO2-N). The catalyst synthesis was accomplished by a sol-gel method using tetrabutyl orthotitanate (C16H36O4Ti), ammonium p-tungstate [(NH4)10H2W12O42·4H2O] and ammonium nitrate (NH4NO3) as the nitrogen source. For comparison, TiO2 and WO3/TiO2 were also prepared under similar conditions. Analysis by X-ray diffraction (XRD), N2 adsorption-desorption, scanning electron microscopy (SEM), transmission electron microscopy (TEM), diffuse reflectance UV-Vis spectroscopy (DRS) and X-ray photoelectron spectroscopy (XPS) were conducted to characterize the synthesized materials. The photocatalytic efficiency of the semiconductors was determined in a batch reactor irradiated with simulated solar light. Residual and mineralized DCF were quantified by high-performance liquid chromatography, total organic carbon analysis and ion exchange chromatography. The results indicated that the tungsten atoms were dispersed on the surface of TiO2 as WO3. The partial substitution of oxygen by nitrogen atoms into the lattice of TiO2 was an important factor to improve the photocatalytic efficiency of WO3/TiO2. Therefore, the best photocatalytic activity was obtained with the WO3/TiO2-N0.18 catalyst, reaching 100% DCF transformation at 250 kJ m-2 and complete mineralization at 400 kJ m-2 of solar-accumulated energy.


Subject(s)
Diclofenac/chemistry , Nitrogen/chemistry , Titanium/chemistry , Adsorption , Catalysis , Microscopy, Electron, Scanning , Microscopy, Electron, Transmission , Oxides , Photochemical Processes , Photoelectron Spectroscopy , Tungsten , X-Ray Diffraction
8.
Environ Sci Pollut Res Int ; 24(14): 12673-12682, 2017 May.
Article in English | MEDLINE | ID: mdl-27832437

ABSTRACT

Photocatalytic degradation of 4-chloro-2-methylphenoxyacetic acid (MCPA) in aqueous solution using Cr(III)-doped TiO2 under UV and visible light was investigated. The semiconductor material was synthesized by a microwave-assisted sol-gel method with Cr(III) doping contents of 0.02, 0.04, and 0.06 wt%. The catalyst was characterized using X-ray powder diffraction (XRD), scanning electron microscopy (SEM), nitrogen physisorption, UV-Vis diffuse reflectance spectroscopy (DRS), and atomic absorption spectroscopy (AAS). The photocatalytic activity for the photodegradation of MCPA was followed by reversed-phase high-performance liquid chromatography (HPLC) and total organic carbon (TOC) analysis. The intermediates formed during degradation were identified using gas chromatography-mass spectrometry (GC-MS). Chloride ion evolution was measured by ion chromatography. Characterization results showed that Cr(III)-doped TiO2 materials possessed a small crystalline size, high surface area, and mesoporous structure. UV-Vis DRS showed enhanced absorption in the visible region as a function of the Cr(III) concentration. The Cr(III)-doped TiO2 catalyst with 0.04 wt% of Cr(III) was more active than bare TiO2 for the degradation of MCPA under both UV and visible light. The intermediates identified during MCPA degradation were 4-chloro-2-methylphenol (CMP), 2-(4-hydroxy-2-methylphenoxy) acetic acid (HMPA), and 2-hydroxybuta-1,3-diene-1,4-diyl-bis (oxy)dimethanol (HBDM); the formation of these intermediates depended on the radiation source.


Subject(s)
Microwaves , Titanium/chemistry , Catalysis , Cresols
9.
Sci Total Environ ; 565: 511-518, 2016 Sep 15.
Article in English | MEDLINE | ID: mdl-27192700

ABSTRACT

The leaching of antimony (Sb) from polyethylene terephthalate (PET) bottling material was assessed in twelve brands of bottled water purchased in Mexican supermarkets by atomic fluorescence spectrometry with a hydride generation system (HG-AFS). Dowex® 1X8-100 ion-exchange resin was used to preconcentrate trace amounts of Sb in water samples. Migration experiments from the PET bottle material were performed in water according to the following storage conditions: 1) temperature (25 and 75°C), 2) pH (3 and 7) and 3) exposure time (5 and 15days), using ultrapure water as a simulant for liquid foods. The test conditions were studied by a 2(3) factorial experimental design. The Sb concentration measured in the PET packaging materials varied between 73.0 and 111.3mg/kg. The Sb concentration (0.28-2.30µg/L) in all of the PET bottled drinking water samples examined at the initial stage of the study was below the maximum contaminant level of 5µg/L prescribed by European Union (EU) regulations. The parameters studied (pH, temperature, and storage time) significantly affected the release of Sb, with temperature having the highest positive significant effect within the studied experimental domain. The highest Sb concentration leached from PET containers was in water samples at pH7 stored at 75°C for a period of 5days. The extent of Sb leaching from the PET ingredients for different brands of drinking water can differ by as much as one order of magnitude in experiments conducted under the worst-case conditions. The chronic daily intake (CDI) caused by the release of Sb in one brand exceeded the Environmental Protection Agency (USEPA) regulated CDI value of 400ng/kg/day, with values of 514.3 and 566.2ng/kg/day for adults and children. Thus, the appropriate selection of the polymer used for the production of PET bottles seems to ensure low Sb levels in water samples.


Subject(s)
Antimony/analysis , Drinking Water/chemistry , Food Contamination/analysis , Polyethylene Terephthalates/chemistry , Water Pollutants, Chemical/analysis , Antimony/chemistry , Food Packaging , Temperature , Water Pollutants, Chemical/chemistry , Water Quality
10.
Photochem Photobiol Sci ; 14(3): 536-42, 2015 Mar.
Article in English | MEDLINE | ID: mdl-25337907

ABSTRACT

In this work, nitrogen-doped ZnO material was synthesized by the sol-gel method using zinc acetate as the precursor and urea as the nitrogen source (15, 20, 25 and 30% wt.). For comparative purposes, bare ZnO was also prepared. The influence of N doping on structural, morphological, optical and photocatalytic properties was investigated. The synthesized catalysts were characterized by XRD, SEM-EDS, diffuse reflectance UV-Vis spectroscopy, BET and XPS analysis. The photocatalytic activity of N-doped ZnO catalysts was evaluated during the degradation of a mixture of herbicides (2,4-D and picloram) under visible radiation ≥400 nm. The photo-absorption wavelength range of the N-doped ZnO samples was shifted to longer wavelength compared to those of the unmodified ZnO. Among different amounts of dopant agent, the 30% N-doped ZnO material showed higher visible-light activity compared with pure ZnO. Several degradation by-products were identified by using HPLC and ESI-MS/MS. The enhancement of visible photocatalytic activity of the N-doped ZnO semiconductor could be mainly due to their capability in reducing the electron-hole pair recombination.


Subject(s)
2,4-Dichlorophenoxyacetic Acid/chemistry , Herbicides/chemistry , Nitrogen/chemistry , Photochemical Processes , Picloram/chemistry , Zinc Oxide/chemistry , Zinc Oxide/chemical synthesis , Catalysis , Chemistry Techniques, Synthetic
11.
Chemosphere ; 121: 68-75, 2015 Feb.
Article in English | MEDLINE | ID: mdl-25434276

ABSTRACT

In this study, a multisyringe chromatography system (MSC) using a C18 monolithic column was proposed for the on-line monitoring of the photocatalytic degradation of isoniazid (INH, 10 mg L(-1)) and pyrazinamide (PYRA, 5mgL(-1)) mixtures in aqueous solution using a small sample volume (200 µL) with an on-line filtration device in a fully automated approach. During the photocatalytic oxidation using TiO2 or ZnO semiconductor materials, total organic carbon (TOC) and the formed intermediates were analyzed off-line using ion chromatography, ion exclusion HPLC, and ESI-MS/MS. The results showed that TiO2 exhibits a better photocatalytic activity than ZnO under UV irradiation (365 nm) for the degradation of INH and PYRA mixtures, generating 97% and 92% degradation, respectively. The optimal oxidation conditions were identified as pH 7 and 1.0 g L(-1) of TiO2 as catalyst. The mineralization of the initial organic compounds was confirmed by the regular decrease in TOC, which indicated 63% mineralization, and the quantitative release of nitrate and nitrite ions, which represent 33% of the nitrogen in these compounds. The major intermediates of INH degradation included isonicotinamide, isonicotinic acid, and pyridine, while the ESI-MS/MS analysis of PYRA aqueous solution after photocatalytic treatment showed the formation of pyrazin-2-ylmethanol, pyrazin-2-ol, and pyrazine. Three low-molecular weight compounds, acetamide, acetic acid and formic acid, were detected during INH and PYRA decomposition. PYRA was more resistant to photocatalytic degradation due to the presence of the pyrazine ring, which provides greater stability against OH attack.


Subject(s)
Antitubercular Agents/isolation & purification , Environmental Monitoring/methods , Isoniazid/isolation & purification , Pyrazinamide/isolation & purification , Water Pollutants, Chemical/isolation & purification , Water Purification/methods , Antitubercular Agents/analysis , Antitubercular Agents/radiation effects , Catalysis , Chromatography, High Pressure Liquid , Environmental Monitoring/instrumentation , Equipment Design , Isoniazid/analysis , Isoniazid/radiation effects , Oxidation-Reduction , Photochemical Processes , Pyrazinamide/analysis , Pyrazinamide/radiation effects , Spectrometry, Mass, Electrospray Ionization , Tandem Mass Spectrometry , Titanium/chemistry , Ultraviolet Rays , Water Pollutants, Chemical/analysis , Water Pollutants, Chemical/radiation effects , Water Purification/instrumentation , Zinc Oxide/chemistry
12.
Sci Total Environ ; 497-498: 153-162, 2014 Nov 01.
Article in English | MEDLINE | ID: mdl-25128885

ABSTRACT

The presence of arsenic (As) in agricultural food products is a matter of concern because it can cause adverse health effects at low concentrations. Agricultural-product intake constitutes a principal source for As exposure in humans. In this study, the contribution of the chemical-soil parameters in As accumulation and translocation in the maize crop from a mining area of San Luis Potosi was evaluated. The total arsenic concentration and arsenic speciation were determined by HG-AFS and IC-HG-AFS, respectively. The data analysis was conducted by cluster analysis (CA) and principal component analysis (PCA). The soil pH presented a negative correlation with the accumulated As in each maize plant part, and parameters such as iron (Fe) and manganese (Mn) presented a higher correlation with the As translocation in maize. Thus, the metabolic stress in maize may induce organic acid exudation leading a higher As bioavailability. A high As inorganic/organic ratio in edible maize plant tissues suggests a substantial risk of poisoning by this metalloid. Careful attention to the chemical changes in the rhizosphere of the agricultural zones that can affect As transfer through the food chain could reduce the As-intoxication risk of maize consumers.


Subject(s)
Arsenic/analysis , Environmental Monitoring , Soil Pollutants/analysis , Zea mays/chemistry , Agriculture , Mexico , Mining , Soil/chemistry
13.
Sci Total Environ ; 488-489: 176-87, 2014 Aug 01.
Article in English | MEDLINE | ID: mdl-24830930

ABSTRACT

Arsenic (As) is a metalloid that may represent a serious environmental threat, due to its wide abundance and the high toxicity particularly of its inorganic forms. The use of arsenic-contaminated groundwater for irrigation purposes in crop fields elevates the arsenic concentration in topsoil and its phytoavailability for crops. The transfer of arsenic through the crops-soil-water system is one of the more important pathways of human exposure. According to the Food and Agriculture Organization of the United Nations, maize (Zea mays L.) is the most cultivated cereal in the world. This cereal constitutes a staple food for humans in the most of the developing countries in Latin America, Africa, and Asia. Thus, this review summarizes the existing literature concerning the conditions involved in agricultural soil that leads to As influx into maize crops and the uptake mechanisms, metabolism and phytotoxicity of As in corn plants. Additionally, the studies of the As accumulation in raw corn grain and corn food are summarized, and the As biotransfer into the human diet is highlighted. Due to high As levels found in editable plant part for livestock and humans, the As uptake by corn crop through water-soil-maize system may represent an important pathway of As exposure in countries with high maize consumption.


Subject(s)
Arsenic/metabolism , Soil Pollutants/metabolism , Zea mays/metabolism , Agriculture , Crops, Agricultural/metabolism , Food Contamination/statistics & numerical data , Soil/chemistry
14.
Talanta ; 99: 730-6, 2012 Sep 15.
Article in English | MEDLINE | ID: mdl-22967617

ABSTRACT

In this work, the potential of a membrane optode coupled to a multisyringe flow injection system (MSFIA) was assessed for determining the Cr(VI) concentration in paint samples. The detection is based on the color obtained from the reaction of Cr(VI) with 1,5-diphenylcarbazide in the presence of sulfuric acid (H(2)SO(4)). The redox product was immobilized on a poly(styrene-divinylbenzene) (SDB-XC) membrane optode. The analyte in the sample was then directly quantified at the surface of the disk by measuring the intensity of reflected incident light using a bifurcated optical fiber at 540 nm. Experimental parameters (concentration of reagents, sample volume, flow rate of sample solutions, eluent concentration, and effect of diverse ions) were studied in detail. The overall time required for the complete procedure was 4 min and only required 0.2 mL of the sample volume. The dynamic working response of Cr(VI) was found within the concentration range of 2.4-1000 µg L(-1) with a limit of detection (LOD) of 0.7 µg L(-1), while the relative standard deviation (RSD) for 400 µg L(-1) Cr(VI) was lower than 2% (n=6). This developed method was used to determine Cr(VI) concentrations in the paint samples, for which an alkaline extraction procedure was proposed. The extraction procedure was based on the use of a 7.5% Na(2)CO(3)/5% NaOH solution at 90 °C for 30 min. Under optimal conditions, the recoveries ranged from 99% to 101%. The complete method was validated using a certified reference material (ERA-QC540, soil sample) and by comparing the results with those obtained using atomic absorption spectrometry (AAS).

15.
Anal Bioanal Chem ; 403(9): 2705-14, 2012 Jul.
Article in English | MEDLINE | ID: mdl-22585054

ABSTRACT

Simultaneous determination of three herbicides (dicamba, 2,4-D, and atrazine) has been achieved by on-line solid-phase extraction (SPE) coupled to multisyringe chromatography (MSC) with UV detection. The preconcentration conditions were optimized; a preconcentration flow rate of 0.5 mL min(-1) and elution at 0.8 mL min(-1) were the optimum conditions. A C(18) (8 mm i.d.) membrane extraction disk conditioned with 0.3 mol L(-1) HCl in 0.5% MeOH was used. A 3-mL sample was preconcentrated, then eluted with 0.43 mL 40:60 water-MeOH. A C(18) monolithic column (25 mm × 4.6 mm) was used for chromatographic separation. Separation of the three compounds was achieved in 10 min by use of 0.01% aqueous acetic acid-MeOH (60:40) as mobile phase at a flow rate of 0.8 mL min(-1). The limits of detection (LOD) were 13, 57, and 22 µg L(-1) for dicamba, 2,4-D, and atrazine, respectively. The sampling frequency was three analyses per hour, and each analysis consumed only 7.3 mL solvent. The method was applied to spiked water samples, and recovery between 85 and 112% was obtained. Recovery was significantly better than in the conventional HPLC-UV method. These results indicated the reliability and accuracy of this flow-based method. This is the first time this family of herbicides has been simultaneously analyzed by on-line SPE-MSC using a monolithic column.


Subject(s)
2,4-Dichlorophenoxyacetic Acid/isolation & purification , Atrazine/isolation & purification , Dicamba/isolation & purification , Herbicides/isolation & purification , Solid Phase Extraction/instrumentation , Water Pollutants, Chemical/isolation & purification , 2,4-Dichlorophenoxyacetic Acid/analysis , Atrazine/analysis , Chromatography, High Pressure Liquid/instrumentation , Dicamba/analysis , Drinking Water/analysis , Equipment Design , Herbicides/analysis , Limit of Detection , Water Pollutants, Chemical/analysis
16.
Environ Technol ; 33(22-24): 2673-80, 2012 Dec.
Article in English | MEDLINE | ID: mdl-23437668

ABSTRACT

The photocatalytic reduction of Cr(VI) from agricultural soil leachates irrigated with Cr(VI)-containing waste hydroponic solution was evaluated in this work. For this purpose, zinc oxide was used as a catalyst under UV irradiation (lambda = 365 nm). The reduction of Cr(VI) was preliminarily evaluated on synthetic solutions with a concentration of 15 mg L(-1) to optimize the catalyst loading and the solution pH and to determine the effect of organic matter. Greater removal of Cr(VI) was observed at pH 7, and the optimum catalyst loading was found to be 2 g L(-1), which achieved an 84% Cr(VI) reduction in 6 h. The influence of dissolved organic matter on the reduction of Cr(VI) was evaluated through the addition of different concentrations of humic acid (HA) to the chromium solution. The removal of Cr(VI) was continuously enhanced as the HA concentration gradually increased from 0 to 14 mg L(-1). The percentage of hexavalent chromium reduction from soil leachates was in the range of 13-99%, and the rate constant was significantly enhanced by the presence of organic compounds in the soil pore water. Thus, a marked synergistic effect between the photocatalytic reduction of Cr(VI) and the organic matter in soil (e.g. humic substances) was observed in real samples and was similar to that observed in the Cr(VI) synthetic solution that contained HA.


Subject(s)
Agriculture , Chromium/chemistry , Soil Pollutants/chemistry , Ultraviolet Rays , Zinc Oxide/chemistry , Catalysis , Hydrogen-Ion Concentration , Oxidation-Reduction , Photochemical Processes , Wastewater
17.
Anal Chim Acta ; 708(1-2): 11-8, 2011 Dec 05.
Article in English | MEDLINE | ID: mdl-22093339

ABSTRACT

In this paper, a novel automatic approach for the speciation of inorganic mercury (Hg(2+)), methylmercury (MeHg(+)) and ethylmercury (EtHg(+)) using multisyringe chromatography (MSC) coupled to cold-vapor atomic fluorescence spectrometry (CV/AFS) was developed. For the first time, the separation of mercury species was accomplished on a RP C18 monolithic column using a multi-isocratic elution program. The elution protocol involved the use of 0.005% 2-mercapthoethanol in 240 mM ammonium acetate (pH 6)-acetonitrile (99:1, v/v), followed by 0.005% 2-mercapthoethanol in 240 mM ammonium acetate (pH 6)-acetonitrile (90:10, v/v). The eluted mercury species were then oxidized under post-column UV radiation and reduced using tin(II) chloride in an acidic medium. Subsequently, the generated mercury metal were separated from the reaction mixture and further atomized in the flame atomizer and detected by AFS. Under the optimized experimental conditions, the limits of detection (3σ) were found to be 0.03, 0.11 and 0.09 µg L(-1) for MeHg(+), Hg(2+) and EtHg(+), respectively. The relative standard deviation (RSD, n=6) of the peak height for 3, 6 and 3 µg L(-1) of MeHg(+), Hg(2+) and EtHg(+) (as Hg) ranged from 2.4 to 4.0%. Compared with the conventional HPLC-CV/AFS hyphenated systems, the proposed MSC-CV/AFS system permitted a higher sampling frequency and low instrumental and operational costs. The developed method was validated by the determination of a certified reference material DORM-2 (dogfish muscle), and was further applied for the determination of mercury species environmental and biological samples.

18.
J Pediatr ; 157(4): 603-9, 609.e1-3, 2010 Oct.
Article in English | MEDLINE | ID: mdl-20542296

ABSTRACT

OBJECTIVE: To determine whether the development of sucking patterns in small-for-gestational age (SGA) preterm infants differs from appropriate-for-gestational age (AGA) preterm infants. STUDY DESIGN: We assessed sucking patterns in 15 SGA and 34 AGA preterms (gestational age

Subject(s)
Child Development/physiology , Infant, Small for Gestational Age , Sucking Behavior , Follow-Up Studies , Gestational Age , Humans , Infant, Newborn , Infant, Premature , Predictive Value of Tests , Surveys and Questionnaires
19.
Anal Chim Acta ; 573-574: 406-12, 2006 Jul 28.
Article in English | MEDLINE | ID: mdl-17723553

ABSTRACT

A novel optical fiber reflectance sensor is coupled to a multisyringe flow injection system (MSFIA) for the preconcentration and determination of 1-naphthylamine (NPA) in water samples using C18 disks (octadecyl groups). NPA, being a first-class carcinogen, is important from a toxicological point of view and, therefore, its quantification is of considerable interest. In this study, the Griess reaction is used for sensitive and selective spectrophotometric determination of NPA. The reaction involves conversion of nitrite into nitrous acid in acidic medium followed by diazotization of sulphanilic acid and formation of a diazonium salt. The diazonium salt is then combined with NPA to form 4-(sulphophenylazo)-1-naphthylamine, an azo dye. This compound is subsequently retained onto a C18 disk followed by spectrophotometric detection at 540 nm, and it is then eluted with methanol in water (80%, v/v), so that the C18 disk is regenerated for subsequent experiments. Under the established optimum conditions, a calibration graph for NPA was constructed. Good linearity was observed within a concentration range from 10 to 160 microg l(-1). The lineal regression equation is A=(0.0027+/-0.0001) [NPA]+(0.0296+/-0.0047), r=0.9991; relative standard deviation values obtained from the analysis of 10 samples of 10, 80 and 160 microg l(-1) are 4.7, 1.2 and 0.6%, respectively. The mean value relative errors for concentrations of 10, 80, 160 microg l(-1) are 3.4, 0.9 and 0.4%, respectively. The detection and quantification limits were 1.1 and 3.7 microg l(-1). A sampling throughput of 14 injections per hour is achieved. The repeatability calculated for five different C18 disks was E(rel)=2.8%. The proposed technique has been validated by replicate analysis (n=6) of several water samples with spiked NPA, giving satisfactory results.

20.
Rev. esp. pediatr ; 51(3): 253-7, 1995. tab
Article in Spanish | CUMED | ID: cum-21470

ABSTRACT

Se presentan algunos aspectos clínicos de 216 pacientes con retraso mental severo y profundo. Hubo un predominio del sexo masculino (59,7 por ciento). La mayor parte de los casos tenían RM profundo (62,5 por ciento). Las causas prenatales de RM ocuparon el primer lugar en frecuencia. El 57,8 por ciento de los pacientes tenían epilépsia, parálisis cerebral infantil o ambas asociadas al RM. Otros déficit asociados como el visual, lenguaje o ambos afectó al 94,4 por ciento de los casos, y los trastornos de conducta al 34, 7 por ciento. Entre las malformaciones, las cardiovasculares fueron las más frecuentes (4,7 por ciento). Los resultados pedagógicos fueron satisfactorios en el 58 por ciento de los pacientes educables, y no satisfactorios en la totalidad de los entrenables. Los resultados obtenidos en la rehabilitación física fueron no satisfactorios en la mayoría de los pacientes


Subject(s)
Humans , Intellectual Disability
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