Ultrasound assisted extraction and spectrophotometric determination of trace selenium in water, food and vegetable samples
2016
Altunay, Nail | Gürkan, Ramazan | Güneş, Murat
In the present study, a new ultrasound assisted extraction (UAE) method was developed for preconcentration of selenite, Se(iv), from sample matrices prior to analysis. The method is based on complex formation between phenoxazine dye, resazurin, and triiodide, I₃⁻, which is produced by oxidation of iodide with Se(iv) in the presence of cetylpyridinium chloride (CPC) at pH 5.0, and then the extraction of the complex into the micellar phase of the extracting agent. The proposed process offers good sensitivity, ease of use and short analysis time. The variables affecting complex formation and extraction efficiency were studied and optimized in detail. Under optimal conditions, a good linear relationship was obtained in the range of 2.5–120 μg L⁻¹ with a detection limit of 0.76 μg L⁻¹. The precision was found to be 3.5% (n: 5, 10 and 40 μg L⁻¹). After preconcentration of a 15 mL sample, a sensitivity enhancement factor of 34.1 was obtained. The method offers good sensitivity, ease of use and short analysis time. Total inorganic Se was determined after the reduction of Se(vi) to Se(iv) using hydrochloric acid. The validation was evaluated by analysis of two standard reference materials (SRMs) and the recovery test. Finally, the method was successfully applied to the determination of inorganic Se in selected samples, and recoveries higher than 93.7% to 103% were obtained.
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