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Biomedical subjects

J Simal-Gándara

Publications and source records attributed to J Simal-Gándara.

At least 19 recordsLinked to original sources

Influence of pH and soil copper on adsorption of metalaxyl and penconazole by the surface layer of vineyard soils.

The upper horizons of old vineyard soils have substantial copper contents due to the traditional use of copper-based fungicides. Total copper levels in eight vineyard soils in the Rías Baixas area of Galicia (northwestern Spain) ranged from 60 to 560 mg kg(-1) (mean +/- SD = 206 +/- 170 mg kg(-1)). The adsorption of the fungicides metalaxyl (pK(a) = 1.41) and penconazole (pK(a) = 2.83) by these soils was determined using fungicide solutions of pH 2.5 and 5.5, and desorption of fungicide adsorbed at pH 5.5 was also determined. In all cases, Freundlich equations were fitted to the data with R (2) > 0.96. Penconazole was adsorbed and retained more strongly than metalaxyl, with K(F) values more than an order of magnitude greater. In the desorption experiments, both fungicides exhibited hysteresis. Soil copper content hardly affected the adsorption of metalaxyl, but K(F) values for adsorption of penconazole increased at a rate of about 0.1 mL(n) (microg of penconazole)(1-n) (microg of Cu)(-1), which is attributed to the formation of Cu(2+)-penconazole complexes with greater affinity for soil colloids than penconazole itself. Because the dependence of K(F) for penconazole adsorption on copper content was the same at both pH values, complex formation appears not to have been affected by the solubilization of 6-17% of soil copper at pH 2.5. A similar copper dependence, or lack of dependence, was observed when 100-1000 mg kg(-1) of copper was added as Cu(NO(3))(2).2H(2)O to the solutions from which the fungicides were adsorbed.

Adsorption↗

Evolution of the concentrations of polycyclic aromatic hydrocarbons in burnt woodland soils.

Little is known of the fate of polycyclic aromatic hydrocarbons (PAHs) in soils under burnt woodland. It is not clear what the behavior of the overlying wood ash layer will be along months. In this study, the levels of eight representative PAHs in the 1-5 cm layer of a periurban woodland soil that had undergone wildfire were compared with those measured in nearby and distant unburnt periurban woodland soils and in a distant unburnt rural woodland soil, and the levels at the burnt site were monitored during some 10 months. The analytical method optimized for the purpose afforded recoveries of 74-111% (depending on PAH) and repeatabilities (RSDs) better than 9%, with limits of detection ranging from 1 to 7 microg/kg. PAH levels in the 1-5 cm layer of the burnt periurban soil were very similar to those of distant unburnt periurban soil (188 vs 173 microg/kg), about seven times the 26 microg/kg measured in unburnt rural soil, which furthermore contained no detectable quantities of the highest molecular weight PAHs typical of traffic and other urban sources, as the periurban soils did. At the burnt site, PAH levels fell along the months (the total PAH level from 188 to 119 microg/kg), apparently as the result of rainfall and the prevention of further input from the atmosphere by the overlying layer of wood ash, which had a very high PAH adsorption capacity (1169 microg/kg) and did not itself appear to act as a source of PAHs. PAH transport may have been assisted by increased mobilization of PAHs associated with dissolvable organic matter due to an increase in soil pH due to alkaline ash components.

Environmental Monitoring↗

Determination of pesticides by solid phase extraction followed by gas chromatography with nitrogen-phosphorous detection in natural water and comparison with solvent drop microextraction.

The European Union specifies that drinking water can contain pesticide residues at concentrations of up to 0.1 microg/L each and 0.5 microg/L in total, and that 1-3 microg/L of pesticides can be present in surface water, but the general idea is to keep discharges, emissions and losses of priority hazardous substances close to zero for synthetic substances. Therefore, in order to monitor pesticide levels in water, analytical methods with low quantification limits are required. The method proposed here is based on solid phase extraction (SPE) followed by gas chromatography with a nitrogen-phosphorous detector (GC-NPD). During method development, six organophosphate pesticides (azinphos-ethyl, chlorfenvinphos, chlorpyriphos, ethoprophos, fenamiphos and malathion) and two organonitrogen pesticides (alachlor and deltamethrin) were considered as target analytes. Elution conditions that could influence the efficiency of the SPE were studied. The optimized methodology exhibited good linearity, with determination coefficients of better than 0.996. The analytical recovery for the target analytes ranged from 70 to 100%, while the within-day precision was 4.0-11.5%. The data also showed that the nature of the aqueous matrice (ultrapure, surface or drinking water) had no significant effect on the recovery. The quantification limits for the analytes were found to be 0.01-0.13 microg/L (except for deltamethrin, which was 1.0 microg/L). The present methodology is easy, rapid and gives better sensitivity than solvent drop microextraction for the determination of organonitrogen and organophosphate pesticides in drinking water at levels associated with the legislation.

Chromatography, Gas↗

Adsorption-desorption dynamics of cyprodinil and fludioxonil in vineyard soils.

Cyprodinil and fludioxonil are new-generation fungicides that are employed to protect grapevines from botrytis and various rots. In this work, their adsorption and desorption dynamics in eight vineyard soils from Galicia (northwestern Spain) were examined in batch and column experiments. Both fungicides exhibited linear adsorption isotherms, with more ready adsorption (greater Kd) of fludioxonil. Kd values for cyprodinil were significantly correlated with soil organic matter content (r 2= 0.675, p < 0.01). Both pesticides exhibited adsorption-desorption hysteresis, but desorption was easier and more variable for cyprodinil (12-21%, RSD = 17%) than for fludioxonil (3-5%, RSD = 13%) and appeared to depend on the formation of irreversible bonds in the former case and on poor solubility in the latter. A linear adsorption model involving nonequilibrium conditions and an irreversible adsorption term was found to reproduce transport behavior accurately.

Adsorption↗

Occurrence of organochlorine pesticides in stream sediments from an industrial area.

Contaminated stream sediments are a serious problem because contaminant residues will be persistent for a long time. Organochlorine pesticides (OCPs) were screened in stream sediments collected along stream flows close to an industrial area in northwestern Spain. Analyses were performed by extraction with organic solvents followed by gas chromatography-mass spectrometry detection. OCPs such as hexachlorobenzene, hexachlorocyclohexane (alpha and beta isomers) and DDT were detected at levels ranging between 29 and 392 microg/kg indicating there is a moderate to severe pollution in the area even though they were banned a few decades ago.

Agriculture↗

Polycyclic aromatic hydrocarbons in smoke from different woods and their transfer during traditional smoking into chorizo sausages with collagen and tripe casings.

Polycyclic aromatic hydrocarbons (PAHs), at least those with high molecular mass, are classified as probable human carcinogens by the US Environmental Protection Agency. The importance of the material used to generate smoke is indicated by the attention that the European Union is paying to list the wood that can be used to produce smoking flavour agents. The paper examines the dependence on the nature of the wood used for smoking on the formation of eight PAHs (selected as markers of PAHs) and transfer of these PAHs into traditional Spanish smoked chorizo sausages with collagen and tripe casings. The results showed that the kind of combustion performed on different materials seriously affected the PAH levels in the smoke generated. Ignition and firing of the material with a flame compared with heating produced more PAHs in the smoke. The levels of PAHs found in the meat and in the collagen and tripe casings of the smoked chorizo samples suggest that the collagen-based casings behave as a better barrier to PAHs.

Chromatography, High Pressure Liquid↗

Determination of polycyclic aromatic hydrocarbons in alcoholic drinks and the identification of their potential sources.

Some polycyclic aromatic hydrocarbons (PAHs), particularly those with a high molecular mass, have been classified as probably being carcinogenic to humans by the International Agency for Research on Cancer (IARC). The significance of the determination of PAHs is reflected by the special attention the European Union is paying to regulating their maximum allowed levels in various types of foodstuffs. Like tobacco and smoked meats, alcoholic drinks can also contain these carcinogenic chemicals, as the latter have been detected in the charred insides of barrels, some ingredients such as caramel or the smoke released during the drying of germinated barley in beer or whisky. This paper determined the contents of seven PAHs in alcoholic beverages of variable alcoholic strength that had been aged in charred barrels for different times (months, years). The aim was to elucidate the dependence of the formation of seven PAHs on the type of charring (traditional or convective) used and the charring intensity (light, medium or heavy). Based on the results, the way the tree raw material is toasted strongly influences PAH levels in alcoholic drinks; thus, traditional charring produces increased amounts of PAHs from the wood relative to convective toasting. The sum of the analysed PAH concentrations in the aged alcoholic beverages studied ranged from zero for a white wine to 172 ng l(-1) for a 'brandy de jerez solera'. The carcinogenic indicator benzo[a]pyrene was found at concentrations below 10 ng l(-1). These PAH concentrations in alcoholic beverages are very low relative to those in smoked and char-broiled foodstuffs. Any health hazards, however, can be minimized by using convective toasting to manufacture the barrels where the drinks are to be aged.

Alcoholic Beverages↗

Comparison of strategies for extraction of high molecular weight polycyclic aromatic hydrocarbons from drinking waters.

Simple, rapid, and inexpensive methods have been developed for the determination of polycyclic aromatic hydrocarbons (PAHs) in drinking waters without interferences from other chemical contaminants by use of two different extraction techniques and analysis by an optimized reverse-phase (RP) high-performance liquid chromatography followed by fluorescence detection (HPLC-FLD) method. The feasibility of SPE (solid-phase extraction) and SPME (solid-phase microextraction) for the determination of PAH in drinking water samples has been evaluated. Several parameters have been studied and optimized for both extraction procedures. The relationship between the nature of the fibers and the quantity of extracted compounds and the effects of organic solvent, salt addition, sampling temperature, and sampling time was studied for SPME. Acetonitrile percentage added to the sample, sample storage conditions (temperature and time), and type of organic elution solvent and elution volume were evaluated for SPE. The results show that both extraction procedures can be used to determine PAHs in drinking waters, but SPE gives better performance (recovery, precision, and quantification limits) for the determination of PAHs in drinking water at the levels established by the legislation.

Chromatography, High Pressure Liquid↗

Procedure to measure the level of polycyclic aromatic hydrocarbons in wood ashes used as fertilizer in agroforestry soils and their transfer from ashes to water.

Before wood ash can be safely used as a fertilizer in soils, possible negative effects such as input of organic contaminants or remobilization of contaminants already stored in the soil must be investigated. The objective of this study was to optimize and characterize extraction methods to isolate and quantitatively measure polycyclic aromatic hydrocarbons (PAHs) concentrations in wood ash that can be used as amendment of soils. It will be then possible to examine the effects of wood ash application on PAHs concentrations in the washing waters with the aim of evaluating their distribution by storage in the different compartments and what influences their stability and persistence. Simple, rapid and inexpensive methods have been set up for the determination of seven polycyclic aromatic hydrocarbons (PAHs) in wood ashes and ash aqueous extracts without interferences from other chemical contaminants using organic solvent extraction and/or SPE techniques and analyzed by an optimized RP-HPLC-FLD method. The feasibility of extraction for the determination of PAHs in wood ashes has been evaluated because PAHs are strongly sorbed to such a matrix, which explains why the PAHs content in ash was seldom studied. The method resulted to be of recoveries ranging from 81 to 97% for the different PAHs, with repeatabilities (RSDs%) better than 6%. Detection levels were from 0.2 to 2.2 microg/kg, while quantification limits were from 0.7 to 5.6 microg/kg, low enough to evaluate the presence of PAHs in wood ashes.

Agriculture↗

Stirring bar sorptive extraction in the determination of PAHs in drinking waters.

The application of a new extraction technique which is known as stir bar sorptive extraction (SBSE), followed by high-performance liquid chromatography with a fluorescence detector, was assessed for determining eight polycyclic aromatic hydrocarbons (PAHs) in water samples. The extraction conditions such as acetonitrile addition; effects of temperature and salt; and finally, extraction and desorption time profiles were studied. Once SBSE was optimized, analytical method parameters such as linearity (r(2)>0.991), precision (<9%), detection (0.5-7.3 ng/L) and quantitation (1.0-22 ng/L) limits were estimated. To correct for the 43-57% absolute recovery depending on the PAH, calibration was done with a line obtained submitting standard-spiked blank tap waters to the complete sample treatment and analysis. Consequently, relative recovery was about 100% because all water samples (those for calibration purposes and those for recovery estimation) were processed in the same way and the absolute recovery remained constant. SBSE method characteristics were checked with the analysis of real drinking waters in the search for PAHs.

Adsorption↗

Application of single-drop microextraction and comparison with solid-phase microextraction and solid-phase extraction for the determination of alpha- and beta-endosulfan in water samples by gas chromatography-electron-capture detection.

Water contamination due to the wide variety of pesticides used in agriculture practices is a global environmental pollution problem. The 98/83 European Directive requires the measurement of pesticides residues at a target concentration of 1.0 microg/l in surface water and 0.1 microg/l in drinking water. In order to reach the level of detection required, efficient extraction techniques are necessary. The application of a new extraction technique: single-drop microextraction (SDME), followed by gas chromatography with electron-capture detection, was assessed for determining alpha-endosulfan and beta-endosulfan in water samples. Experimental parameters which control the performance of SDME, such as selection of microextraction solvent and internal standard, optimization of organic drop volume, effects of sample stirring, temperature and salt addition, and sorption time profiles were studied. Once SDME was optimized, analytical parameters such as linearity, precision, detection and quantitation limits, plus matrix effects were evaluated. The SDME method was compared with solid-phase microextraction and solid-phase extraction with the aim of selecting the most appropriate method for a certain application.

Chromatography, Gas↗

HPLC method for determining ethylenediamine migration from epoxy-amine food packaging coatings into EU food simulants.

A simple, rapid, sensitive and inexpensive method has been developed for the determination of ethylenediamine (EDA) in European Union food simulants. The method involves precolumn derivatization with ortho-phthaldehyde (OPA) and 2-mercaptoethanol (ME) to obtain a fluorescent derivative. Liquid chromatographic (HPLC) elution was achieved with methanol-ultrapure water (65:35) as mobile phase with a Waters Spherisorb 5 microm ODS 2 column. Fluorescence detection (FD) was performed at 330 nm (excitation wavelength) and 450 nm (emission). Total chromatographic analysis time was < 10 min. The proposed method was validated by checking linearity, detection and quantification limits, and precision. Relative recovery rates were of about 100% because samples and standard-spiked blanks were processed in the same way. Method precision (RSD < 6%) was satisfactory and the quantification limit (0.25 mg x (-1)) indicated that specific migration limit for EDA in EU food simulants (12 mg x kg(-1)) can be easily controlled. When the validated method was applied to epoxy-amine formulations used for can coatings under different curing conditions, EDA migration was < 1.4 mg x l(-1).

Acetic Acid↗

Analytical methods for food-contact materials additives in olive oil simulant at sub-mg kg-1 level.

Methods of analysis for four additives (two antioxidants, IRGANOX 245 and 1035; an ultraviolet absorber, CHIMMASORB 81; and an optical brightening agent, UVITEX OB) in olive oil are reported. These additives have the potential to migrate from food-contact materials into the European Union fatty food simulant olive oil, which is the most difficult matrix for analysis. The additives were chosen because they differed in their chemically active groups, had different functions within the polymer, have low proposed specific migration limits and are commonly used in food-contact materials such as polystyrenes and polyolefins. The proposed analytical methods for the additives are simple, rapid, inexpensive and also broadly applicable to the aqueous food simulants. All methods were evaluated by constructing calibration curves, measurement of recovery and precision, and determining the limits of detection. Most of the methods involve direct injection of an olive oil solution for high-performance liquid chromatography analysis with ultraviolet-visible or fluorescence detection. The methods allowed establishment of additive stability and measurement of migration of the selected additives into olive oil at different time-temperature conditions used in migration studies into food simulants.

Antioxidants↗

Optimization of solid-phase extraction and solid-phase microextraction for the determination of alpha- and beta-endosulfan in water by gas chromatography-electron-capture detection.

Water contamination due to the wide variety of pesticides used in agriculture practices is a global environmental pollution problem. The 98/83/European Directive requires to measure residues of pesticides at a target concentration of 1.0 microg/l in surface water and 0.1 microg/l in drinking water. In order to reach the level of detection required, efficient extraction techniques are required. Although solid-phase extraction (SPE) is the most common technique for isolation and concentration of pesticides from water, solid-phase microextraction (SPME) is being increasingly applied for this purpose. In this study, a direct-SPME procedure has been developed for the determination of alpha-endosulfan and beta-endosulfan in waters; experimental parameters such as selection of SPME coating, effect of temperature, effect of salt addition, optimization of the sample volume, adsorption and desorption profiles and desorption temperature were studied and optimized. Analytical parameters such as linearity, precision, detection and quantitation limits, and matrix effects for SPE and SPME methods were evaluated for comparison purposes with the aim of selecting the most appropriate for a certain application. Both extraction techniques, SPE and SPME, were followed by gas chromatography with electron-capture detector.

Chromatography, Gas↗

Comparison of solid-phase extraction and solid-phase microextraction for carbofuran in water analyzed by high-performance liquid chromatography-photodiode-array detection.

In this study a direct solid-phase microextraction (SPME) procedure has been developed for the determination of carbofuran in water. Experimental parameters such as selection of SPME coating, effect of temperature, effect of salt addition and solvent desorption were studied and optimized. Analytical parameters such as linearity, precision, detection and quantitation limits, and matrix effects for solid-phase extraction (SPE) and SPME methods were evaluated for comparison purposes with the aim of selecting the most appropriate depending on the detection capabilities required. SPE and SPME were followed by high-performance liquid chromatography with diode-array detection, using a 50 x 4.6 mm I.D. guard column and a 150 x 4.6 mm I.D. analytical column, both packed with C18 silica. Both methods can be applied to real samples and give the same results, but SPE allows the detection of lower carbofuran concentrations (0.06 microg/L) as compared to

Carbofuran↗

Tests of potential functional barriers for laminated multilayer food packages. Part II: Medium molecular weight permeants.

Experiments were performed to characterize the kinetics of the permeation of different medium molecular weight model permeants: bisphenol A, warfarin and anthracene, from liquid paraffin, through a surrogate potential functional barrier (25 microns-thick orientated polypropylene--OPP) into the food simulants olive oil and 3% (w/v) acetic acid. The characterization of permeation kinetics generally observed the permeation models previously reported to explain the experimental permeation results obtained for a low molecular weight group of model permeants. In general, the model permeants exhibited behaviour consistent with their relative molecular weights with respect to (a) the time taken to attain steady-state permeation into the food simulant in which they were more soluble, (b) their subsequent steady-state permeation rates, and (c) their partition between liquid paraffin and the OPP membrane.

Acetic Acid↗