Biomedical subjects

Pilar Ortega-Barrales

Publications and source records attributed to Pilar Ortega-Barrales.

4 recordsLinked to original sources

PubMed2005

Rapid determination of diphenylamine residues in apples and pears with a single multicommuted fluorometric optosensor.

In this work, a single flow injection multicommuted system using solid-surface fluorescence spectroscopy has been explored for the determination of diphenylamine in apples and pears. The native fluorescence signal of diphenylamine retained on the solid support (C18 silica gel) was used for its determination (lambda(exc)/lambda(em) 291/372 nm). The sample treatment consists of a liquid-liquid extraction with acetonitrile followed by a cleanup step using primary-secondary amines. The use of a continuous flow assembly implementing multicommutation, based on a set of three-way solenoid valves controlled by appropriate software, provides the automatic control of sample, carrier, and eluting solution with remarkable advantages in relation to conventional flow injection approaches. Using an optimized sampling time, the proposed method was linear in the range 0.25-5 mg kg(-1) with a detection limit of 0.06 mg kg(-1) and RSD (percent) values better than 3%. The proposed method was successfully applied to the analysis of diphenylamine in different apple and pear samples fortified at different concentrations, and recoveries between 78 and 104% were found. The results obtained illustrate the usefulness of the proposed method for the screening and evaluation of postharvest treatment of crops possibly containing diphenylamine.

Diphenylamine↗

PubMed2004

Development of a single fluorescence-based optosensor for rapid simultaneous determination of fungicides benomyl and thiabendazole in waters and commercial formulations.

A novel, sensitive, and straightforward spectrofluorimetric flow injection method is proposed in this work for the resolution of a binary mixture of two widely used fungicides (thiabendazole and benomyl). The continuous flow methodology is based on the implementation of on-line solid phase extraction (SPE), preconcentration, and separation of both analytes on a surface of C(18) silica gel beads placed just in the flow cell, with solid surface fluorescence detection. A 45- and 25-fold sensitivity enhancement was obtained for benomyl and thiabendazole, respectively (in relation to the liquid phase measurements in the absence of solid support). The separation of the pesticides was performed because of the different retention-desorption kinetics in their interaction with the solid support, in the zone where the stream impinges the solid material. No previous separation of the analytes before they reach the flow cell is needed, simplifying extraordinarily both the procedure and the manifold. Using a sample volume of 3200 microL, the system was calibrated in the range of 0.4-20 and 20-400 ng x mL(-)(1) with detection limits of 0.06 and 3.6 ng x mL(-)(1) for thiabendazole and benomyl, respectively, and RSD values (n = 10) smaller than 0.8% for both analytes. The RSD values obtained replacing the solid support in each measurement were lower than 3%, and the day-to-day reproducibility RSD value was also lower than 5%. Sampling frequencies of 10 and 18 h(-)(1) were obtained with 600 and 3200 microL of sample volume. Recovery studies carried out on natural water samples spiked with known amounts of both analytes at concentration levels in the range of 1-10 and 25-200 ng x mL(-)(1) provided mean recovery percentages ranging from 98.8 to 102% and from 98 to 103% for thiabendazole and benomyl, respectively. The proposed methodology was also applied to pesticide formulations.

Benomyl↗

PubMedDate not supplied

Use of a continuous flow solid-phase spectroscopic sensor using two sensing zones: determination of thiamine and ascorbic acid.

A simple, rapid, inexpensive, and automated flow-through solid-phase spectroscopic sensing device is proposed for the sequential determination of 2 vitamins: thiamine and ascorbic acid. The vitamins are concentrated on ion-exchange gels, thiamine on Sephadex SP C-25, and ascorbic acid on Sephadex QAE A-25; both solid supports are packed in 2 different flow cells. The absorbance is monitored directly on the solid phase with a double-beam spectrophotometer at 250 nm, without derivatization or additional elution. With the use of 2 carrier/self-eluting solutions (0.1 5M sodium acetate/acetic acid and 0.18M citric acid/K2HPO4) and a sample volume of 1000 microL, the sensor responds linearly in the range of 0.5-15 and 3-50 microg/mL with detection limits of 0.14 and 0.36 microg/mL for thiamine and ascorbic acid, respectively. When the method was applied to synthetic samples and pharmaceutical preparations, precise and accurate values were obtained.

Ascorbic Acid↗

PubMedDate not supplied

Flow-through fluorescence-based optosensor with on-line solid-phase separation for the simultaneous determination of a ternary pesticide mixture.

A rapid and selective method was developed for the simultaneous determination of 3 widely used pesticides, carbendazim (CBZ), carbofuran (CF), and benomyl (BNM). The method utilized a single continuous-flow, solid surface fluorometric multioptosensor implemented with a previous separation of the analytes on a minicolumn, placed just before the sensor, that was packed with the same solid support (C18 silica gel) as the flow-through cell. The separation was achieved because of the different kinetics of retention/elution of the pesticides on the solid support in the minicolumn, enabling the sequential arrival of the analytes at the sensing zone. With a single injection of the mixture, 2 of them were more strongly retained in the minicolumn (CF and BNM) while the other (CBZ) passed through the system towards the sensing material where it developed its fluorescence transitory signal. Then, CF and BNM were successively eluted from the solid support using 2 different eluting solutions, and they sequentially reached the sensing zone and developed their respective signals. A multiwavelength fluorescence detection mode was used, recording the signals of each pesticide at its maximum excitation/emission wavelength; therefore, the sensitivity was increased. The system was calibrated using a sample volume of 2000 microL. The linear dynamic range was 80-1400, 250-2400, and 150-2000 ng/mL with detection limits of 15, 68, and 35 ng/mL and relative standard deviation values of 3.5, 3.2, and 2.4% for CBZ, CF, and BNM, respectively. A recovery study was applied to spiked environmental water samples, and recoveries ranged from 96 to 104%.

Air Pollutants, Occupational↗