No abstract

No abstract

No abstract

No abstract

No abstract

<p>A new analytical approach was developed involving mag-netic solid-phase extraction (MSPE) and spectrofluorimetric determi-nation of propranolol (PRO) in biological fluids. A urine or plasma sample was prepared and adjusted to pH 3-4, then PRO was quickly</p>extracted using Fe3O4 magnetic nanoparticles (MNPs) modified by the surfactant sodium dodecyl sulfate (SDS) and determined applying spectrofluorimetry. Experimental conditions, such as the amount of MNPs and SDS, pH value, standing time, desorption solvent and maximal extraction volume have been adjusted to optimize the extraction process and to obtain analytical characteristics of the method. Linearity was observed in the analyte’s concentration range of 2-75 ng mL-1 for both urine and plasma samples. The correlation coefficients (r) were higher than 0.99. The method showed good precision and accuracy, with intra- and inter-assay precisions of less than 5.0% at all concentrations. Standard addition recovery tests were carried out, and the recoveries ranged from 79.4% to 90.4%. The limits of detection and quantification were 0.85 and 2.80 ng mL-1, respectively, for urine and 0.74 and 2.43 ng mL-1, respectively, for plasma. The method was applied to the determination of PRO in human urine and plasma samples.

A simple, rapid and sensitive spectrofluorimetric method was developed for the determination of di-syston, ethion and phorate in environmental water samples. The procedure is based on the oxidation of these pesticides with cerium (IV) to produce cerium (III), and its fluorescence was monitored at 368 ± 3 nm after excitation at 257 ± 3 nm. The variables effecting oxidation of each pesticide were studied and optimized. Under the experimental conditions used, the calibration graphs were linear over the range 0.2-15, 0.1-13, 0.1-13 ng mL(-1) for di-syston, ethion and phorate, respectively. The limit of detection and quantification were in the range 0.034-0.096 and 0.112-0.316 ng mL(-1), respectively. Intra- and inter-day assay precisions, expressed as the relative standard deviation (RSD), were lower than 5.2 % and 6.7 %, respectively. Good recoveries in the range 86 %-108 % were obtained for spiked water samples. The proposed method was applied to the determination of studied pesticides in environmental water samples.

Two new methods based on cloud point extraction (CPE) technique were developed and optimized for the extraction and preconcentration of oxazepam from human urine, as an azo or fluorescent derivative. The first method is a spectrophotometric one, which is based on the acid hydrolysis of the oxazepam to a benzophenone, diazotization of the benzophenone, and then the coupling with oxine to form an azo dye. The second method is a spectrofluorimetric one, which involves reduction of the target compound using Zn°/HCl at room temperature with the formation of a highly fluorescent derivative. The main factors affecting the chemical reactions and CPE were investigated and optimized systematically. Under optimum experimental conditions, the calibration graphs were linear in the range of 0.1 to 1.5 (0.05 to 2.0) µg/ml with correlation coefficients of 0.9989 (0.9985), for the CPE-spectrophotometric (CPE-spectrofluorimetric) method. The limit of detection was found to be 0.034 (0.018) µg/ml and the relative standard deviation was calculated to be 1.35 (2.52)%. Recoveries in the spiked samples ranged from 87 to 94%. Finally, the proposed methods were applied to the determination of oxazepam in human urine.