Biomedical subjects

E Rodríguez-Gonzalo

Publications and source records attributed to E Rodríguez-Gonzalo.

11 recordsLinked to original sources

PubMed2006

Determination of endocrine-disrupting compounds in cereals by pressurized liquid extraction and liquid chromatography-mass spectrometry. Study of background contamination.

A sensitive method based on pressurized liquid extraction (PLE) and liquid chromatography-electrospray ionization mass spectrometry (LC-ESI-MS) has been developed for the determination in cereal samples of seven endocrine-disrupting compounds: bisphenol A (BPA), 4-tert-butylbenzoic acid (BBA), 4-nonylphenol (NP), 4-tert-butylphenol (t-BP), 2,4-dichlorophenol (DCP), 2,4,5-trichlorophenol (TCP) and pentachlorophenol (PCP). For the PLE procedure, methanol was selected as the extraction solvent. An experimental design approach was applied to optimize other PLE parameters. The recoveries achieved for the all seven compounds were in the 81-104% range, with relative standard deviations of 4-9%. An additional preconcentration step, based on solid-phase extraction (SPE), after the PLE step proved to be a successful way for obtaining a more sensitive method. The detection limits achieved in corn breakfast cereals were in the 0.003-0.013 microg g(-1) range, except for BPA, with a detection limit of 0.043 microg g(-1), for a sample size of 2.5 g. These values are similar to or even lower than currently legislated limits for pesticides in cereals and cereal-based foodstuffs. We also investigated possible contamination during the experimental process by the target compounds released from purified water, plastics, syringes, peristaltic pump tubes, glassware and other laboratory materials in contact with the samples along the analytical process.

Analytic Sample Preparation Methods↗

PubMed2006

Comparison of a non-aqueous capillary electrophoresis method with high performance liquid chromatography for the determination of herbicides and metabolites in water samples.

A method of capillary electrophoresis (CE) for the determination of triazine herbicides and some of their main metabolites in water samples has been developed. The proposed CE method includes an off-line solid-phase extraction (SPE) procedure with LiChrolut EN sorbent coupled to a non-aqueous capillary electrophoresis (NACE) separation with UV detection. The target compounds were the chloro-s-triazines simazine, atrazine, propazine; the methyltio-s-triazines ametryn and prometryn and three main derivatives from the atrazine degradation products; namely, deethylatrazine, deethylhydroxyatrazine and deisopropylhydroxyatrazine. The analytical characteristics of the CE method are reported. The repeatability of the method was studied considering the different steps of the method separately in order to determine the contributions of each step to the total variability of the method. The NACE-UV results are compared with those obtained with a high performance liquid chromatography with UV detection (HPLC-UV) method. The same off-line SPE procedure was applied to both techniques. The results obtained show that both methods afford the same results in the analysis of surface and drinking water samples, with a level of significance regarding the F- and t-tests greater than 0.05 in all the cases. The detection limits in surface water samples were in the 0.04-0.32 microg l(-1) and 0.11-1.2 microg l(-1) ranges for the NACE-UV and HPLC-UV methods, respectively. The recoveries (spiked/found) were significantly 100% in all cases.

Atrazine↗

PubMed2005

Pressurized liquid extraction in the analysis of food and biological samples.

Originally, the use of the pressurized liquid extraction technique (PLE) was mainly focused on the extraction of environmental pollutants present in soil matrices, sediments, and sewage sludge. However, more recently the distinct advantages of this technique are being exploited in diverse areas, including biology, and the pharmaceutical and food industries. The aim of the present review is to explore recent analytical applications of this extraction technique (PLE) in the extraction of contaminant compounds and matrix components in food and biological samples, placing special emphasis on the strategies followed to obtain a rapid, selective, efficient and reliable extraction process.

Chromatography, Liquid↗

PubMed2005

Determination of triazines and dealkylated and hydroxylated metabolites in river water using a propazine-imprinted polymer.

A molecularly imprinted polymer (MIP) obtained by precipitation polymerisation using propazine as template has been employed as sorbent for the solid phase extraction of triazines and some of their hydroxylated and dealkylated metabolites from river water. Three configurations were studied: (a) use of the propazine-MIP as a selective sorbent for the extraction of triazines directly from water; (b) use of mixtures of LiChrolut EN (a polymeric sorbent of styrene divinylbenzene) and propazine-MIP as sorbent, and (c) use of propazine-MIP as a clean-up sorbent for organic extracts obtained in a prior SPE procedure with LiChrolut EN. The former two configurations imply that the analytes pass through the propazine-MIP in aqueous medium, whereas in the latter case the analytes percolate through the propazine-MIP in an organic medium coming from the previous SPE step. Different types of water were tested to assess matrix effects. The analytical characteristics of the three configurations were evaluated.

Alkylation↗

PubMed2004

Determination of weakly acidic endocrine-disrupting compounds by liquid chromatography-mass spectrometry with post-column base addition.

A sensitive analytical method based on liquid chromatography-electrospray ionisation mass spectrometry (LC-ESI-MS) has been developed for the determination of seven endocrine-disrupting compounds: 4-n-nonylphenol (NP), 4-tert-butylphenol (t-BP), bisphenol A (BPA), 2,4-dichlorophenol (DCP), 2,4,5-trichlorophenol (TCP), pentachlorophenol (PCP) and 4-tert-butylbenzoic acid (BBA) in water samples. To achieve a good LC separation, acidification of the LC mobile phase was necessary, but this led to MS signal suppression for the less acidic compounds. In order to enhance the sensitivity for these analytes, post-column addition of different bases such as ammonia, trimethylamine, and 1,8-diazabicyclo-(5,4,0)undec-7-en (DBU) was evaluated. The post-column addition of base is proposed here to raise effluent pH, helping in the ionisation process of the compounds with higher pKa values (t-BP, BPA, DCP and NP). The use of DBU, diluted in MeOH, proved to be the most efficient post-column reagent for enhancing the MS signal. The signal-to-noise ratios for t-BP and NP increased by more than 200-fold and 35-fold, respectively, whereas for DCP and BPA an increase of about 10-fold was achieved. This strategy permitted direct determination of the seven compounds at low ppb levels. For application to real water samples, an extraction and preconcentration step using the solid-phase extraction (SPE) technique was carried out. The applicability of three solid-phase materials--Bond Elut C18, and two polymeric sorbents: LiChrolut EN and Oasis HLB--and the optimization of other SPE parameters such as the elution solvent and sample volume used, were studied in order to maximize extraction efficiency. Oasis HLB provided the best results, obtaining--with the proposed SPE procedure--satisfactory percentage recoveries for all compounds (70-110%) with the exception of NP, for which a recovery of 54% was achieved. Application of the whole method, SPE-LC-(ESI)-MS, to natural waters permitted low nanogram-per-liter determination of all seven compounds.

Acids↗

PubMed2003

Prediction of the behaviour of organic pollutants using cloud point extraction.

A preconcentration study based on the cloud point phenomenon was carried out for a set of triazine herbicides, three of them chloro-substituted and three of them methylthio-substituted. Concentration factors and recoveries were calculated as function of the percentage of the non-ionic surfactant Triton X-114 employed. From these values, obtained from a cloud point extraction (CPE) procedure, the distribution coefficient between the Triton X-114 micelles and water, Kc, prior to CPE was calculated for each triazine and related to the corresponding octanol-water partition coefficient, Kow. In order to confirm the results obtained with the triazine herbicides, two sets of data from chemically different organic pollutants--organophosporous and chlorophenols--obtained from the literature were assessed, concluding that they display a similar behaviour to that of the triazine herbicides. This can be used to predict the CPE behaviour of other organic pollutants from their octanol-water partition coefficients. The Kc values were compared with the analyte concentration ratio in the surfactant-rich phase and aqueous phase (Ksa) with a view to obtaining a link between the analyte behaviour prior to and after cloud point extraction procedures.

Environmental Pollutants↗

PubMed2003

Determination of herbicides, including thermally labile phenylureas, by solid-phase microextraction and gas chromatography-mass spectrometry.

A method for the determination of 10 herbicides, including thermally unstable compounds, has been developed. The method uses solid-phase microextraction (SPME) with a polyacrylate fibre. Separation, identification and quantification were accomplished with gas chromatography-mass spectrometry. The herbicides chosen belong to different chemical groups and were alachlor, atrazine, chlorotoluron, diclofop, diflufenicam, ethofumesate, isoproturon, linuron, terbutryn and trifluralin. In the present work we studied the chromatographic behaviour of three phenylureas as a function of the medium and injection mode employed. The compounds generated as a function of the solvent used in direct injection of the phenylureas (ethyl acetate, methanol and methanol-water) and those obtained when injection was accomplished using the polyacrylate fibre were determined. The results allow us to propose a method for the determination of stable and thermally unstable herbicides as long as a preconcentration step involving SPME is carried out. In the proposed method, the limits of detection varied between 0.02 microg/l for ethofumesate and 0.11 microg/l for chlorotoluron. The method was applied to the determination of these herbicides in surface and ground water samples, performing quantification by standard addition calibration. The contents of chlorotoluron and atrazine found were significantly equal to those obtained using HPLC after a preconcentration stepwith styrene-divinylbenzene sorbents.

Gas Chromatography-Mass Spectrometry↗

PubMed2003

Solid-phase extraction and sample stacking-micellar electrokinetic capillary chromatography for the determination of multiresidues of herbicides and metabolites.

Micellar electrokinetic capillary chromatography (MEKC) with diode array detection was used for the separation of 13 compounds (eight herbicides widely used in agriculture: metribuzin, lenacil, ethofumesate, atrazine, terbutryn, isoproturon, chlorotoluron and linuron, and five of their principal degradation products; namely, deethylatrazine, 2-hydroxyatrazine, deethyl-2-hydroxyatrazine, deisopropylatrazine and 3-chloro-4-methylphenylurea). Peak separation for the 13 analytes was not successful when a single surfactant system was employed, neither sodium dodecyl sulfate (SDS) nor dioctyl sulfosuccinate (DOSS) sodium salt. However, a mixture of these herbicides was successfully separated using a mixed micellar system involving SDS-DOSS in less than 14 min. An application study of an on-line concentration technique for MEKC was carried out to enhance sensitivity. The optimized on-line stacking procedure consisted simply of the addition of 50 mM of sodium chloride to the injection sample, the stacking effect being more intensive as analyte polarity increased. When this stacking procedure was combined with an off-line sample preconcentration step, based on solid-phase extraction, analytes could be detected in the ppb range. The whole method was applied to ultra-high-quality and natural waters. Linear relationships between the analytical signal and the initial analyte concentration were found to be independent of the type of water, except for the more polar analytes for which small differences were observed.

Chromatography, Micellar Electrokinetic Capillary↗

PubMed2000

Surfactant cloud point extraction and preconcentration of organic compounds prior to chromatography and capillary electrophoresis.

The use of preconcentration steps based on phase separation by the cloud point technique offers a convenient alternative to more conventional extraction systems. It has been used successfully for the preconcentration of species of widely differing character and nature, such as metal ions, proteins and other biomaterials, or organic compounds of strongly differing polarity. Here we address the most recent analytical applications of this methodology when used as an isolation and trace enrichment step prior to the analysis of organic compounds (polycyclic aromatic hydrocarbons, polychlorinated compounds, pesticides, phenolic derivatives, aromatic amines, vitamins, etc.) via liquid and gas chromatography or capillary electrophoresis.

Chemical Phenomena↗

PubMed2000

Analysis of pesticide residues in matrices with high lipid contents by membrane separation coupled on-line to a high-performance liquid chromatography system.

Separation through membranes coupled to an HPLC system was used as a technique for the analysis of pesticide multiresidues in samples with high lipid contents. As well as the usual procedure, in the proposed system it is possible to recirculate the sample through the membrane cell, which permits the extraction system to be applied to cases in which only a very small volume of sample is available. A procedure for pesticide multiresidue analysis in egg samples was developed as a representative example of the applicability of the proposed method. To accomplish this, the analytes (dichlorvos, dimethoate, propoxur, paraoxon, pirimicarb, atrazine, ametryne, terbutryne, azinphos-methyl, folpet) were subjected to prior extraction in a Soxhlet system, after which the extract was introduced into the membrane separation device coupled to the HPLC system. This procedure afforded clean chromatograms, hence considerably facilitating determination, and at the same time was efficient in removing macromolecular compounds. For egg samples, spiked at a concentration level of 0.750 mg/kg, recoveries ranged from 60 to 98%. The detection limits varied from 0.018 mg/kg for dichlorvos to 0.002 mg/kg for atrazine.

Chromatography, High Pressure Liquid↗

PubMed2000

Determination of triazine herbicides in natural waters by solid-phase extraction and non-aqueous capillary zone electrophoresis.

Capillary zone electrophoresis (CZE) in an organic medium was used to analyse triazines at sub-ppb concentration levels in natural waters after a preconcentration step using conventional C18 cartridges and new Oasis HLB devices. With both sorbents, satisfactory results were obtained on analysing deionized water. However, on analysing natural waters, both sorbents showed very different types of behaviour. The different variables affecting the elution of both sorbents were studied, resulting in the choice of Oasis HLB as the most suitable for later separation by CZE in non-aqueous medium. Combination of a preconcentration step with electrokinetic injection revealed that capillary electrophoresis with simple UV detection can also be used satisfactorily for the quantification of micropollutants in natural waters. The detection limits obtained varied between 0.01 and 0.05 microg l(-1), depending on the type of matrix analysed. The day-to-day precision varied between 0.9% and 2.3%, expressed as the relative standard deviation.

Electrophoresis, Capillary↗