A rapid method for speciation and determination of organomercury compounds in biological samples of marine origin using Capillary Electrophoresis (CE) is reported. Organomercurials were extracted from the samples by means of the classical Westöö procedure thus giving organomercury-cysteine complexes which can be separated from each other by means of CE resulting in effective speciation. Electrophoretic separation was achieved in an open silica capillary tube at 15-18 kV using a 100mM sodium borate buffer (pH 8.35). All mercury species were distinctively separated within 12 min. Results are presented for the analysis of real marine samples and reference materials, and compared with those obtained by the GC commonly accepted procedure.
A simple and rapid dispersive liquid-liquid microextraction method has been developed for the determination of 11 benzotriazoles and benzothiazoles in water samples. Tri-n-butylphosphate (TBP) was used as extractant, thus avoiding the use of toxic water-immiscible chlorinated solvents. The influence of several variables (e.g., type and volume of dispersant and extraction solvents, sample pH, ionic strength, etc.) on the performance of the sample preparation step was systematically evaluated. Analytical determinations were carried out by high-performance liquid chromatography with fluorescence and UV detection and liquid chromatography-electrospray ionization-tandem mass spectrometry. The optimized method exhibited a good precision level with relative standard deviation values between 3.7% and 8.4%. Extraction yields ranging from 67% to 97% were obtained for all of these considered compounds. Finally, the proposed method was successfully applied to the analysis of benzotriazoles and benzothiazoles in real water samples (tap, river, industrial waters, and treated and raw wastewaters).
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