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A sensitive, simple and rapid method for ultra-trace determination of iron and manganese based on ultrasound assisted pseudodigestion in citric acid fermentation medium samples (beet and cane molasses and raw sugar based mediums) is described. Parameters influencing pseudo-digestion, such as sonication time, sample mass and solvent system were fully optimized. Final solutions obtained upon sonication were analyzed by electrothermal atomic absorption spectrometry (ETAAS). The best conditions for metal pseudo-digestion were as follows: a 25, 30 and 20 min sonication time for beet molasses, cane molasses and raw sugar based medium samples, respectively, 0.7 g sample mass of raw sugar based samples, 0.5 g sample mass of molasses based samples and an extraction mixture of concentrated HNO3-H2O2, in 25 mL of solvent. Analytical results obtained for the two metals by ultrasound assisted pseudo-digestion and conventional wet digestion methods showed a good agreement. This method reduces the time required for all treatments (heating to dryness, cooling and separation) in comparison with conventional wet digestion method. The accuracy of the method was tested by comparing the obtained results with that of conventional wet digestion method. [...]
EN
The parameters of analytical procedures developed for direct ETAAS determination of Pb in wine are discussed. Atomic absorption spectrometers based on transversal and longitudinal Zeeman effect, wall and integrated platform atomization with two main approaches: (i) measurements in the presence of modifier and (ii) measurements without using any modifier are compared. The optimal temperature programs are defined according to the pre-treatment and atomization curves constructed in the presence of different types of wines. For all investigated instrumental systems, 1:1 dilution of wine sample with 0.2 mol L−1 HNO3 is recommended. Matrix interferences observed, call for standard addition calibration method for Pb quantification in wines. The detection limit (3σ) achieved for wine diluted in the ratio of 1:1 varied from 0.8 to 1.9 μg L−1 depending on the instrument used. The relative standard deviation for the concentration range of 10 to 80 μg L−1 Pb in wine is typically between 4–8%. The accuracy of the analytical procedures recommended was confirmed by comparing the results obtained with those found for wine samples previously digested with HNO3-H2O2 mixture, by added/found method and by parallel analysis using different instruments. A total of 66 wine samples from different regions of Macedonia were analyzed. [...]
EN
Abstract Cis-diamminedichloroplatinum(II) (cisplatin) was immobilized in a star-shaped polymer carrier. In order to define whether this polymer could be used as a drug delivery system for cisplatin, its characteristics, e.g. loading efficiency and release profile of cisplatin from the polymer in phosphate buffered saline (PBS), have to be assessed, and hence an appropriate analytical procedure for precise and reliable determination of Pt(II) must be established. Optimal instrumental parameters for Pt measurement by commonly used atomic spectrometric methods ETAAS and ICP-OES in various examined media were defined. Matrix interferences observed that were related to both techniques were evaluated, and analytical figures of merit were compared and critically discussed. Graphical abstract [...]
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