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Evaluation of sample treatment in micro-scale for determination of Ca, Cu, Fe, K, Mg, Na and Zn in sausage by MIP OES
Anderson Schwingel Ribeiro
Universidade Federal de Pelotas
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Crie um tópicoSausage is an industrialized meat product obtained from the emulsion of beef, pork or poultry and edible offals, which attribute various nutrients and essential elements. During their processing, many sodium-based additives are used, which are responsible for preserving the food and enhancing the flavor, making the sausage a risky food for the population when consumed in excess due to the high concentrations of this element. In addition, the presence of elements that are beneficial to health, but in excess, can cause several disturbances in the physiological system. Due to the complexity of the sausage sample matrix, rich in fat, it is necessary studies for the correct sample preparation for analysis, to obtain accurate and precise results. The literature reports several methods for biological samples, which most often use large quantities of samples and reagents, associated with heating at high temperatures. Therefore, the micro-scale method is attractive, because in addition to reducing the amount of sample for analysis, it consumes lower volume of reagents, generating a smaller amount of waste, reducing the analysis time and offering greater security for the analyst. Thus, this study aimed to evaluate the acidic decomposition method in micro-scale, using mini vessels made of polytetrafluoroethylene (PTFE) for sample preparation in a closed system with microwave heating for determination of Ca, Cu, Fe, K, Mg, Na and Zn in sausage samples. The determinations were performed by microwave-induced plasma optical emission spectrometry (MIP OES) technique. The method developed was based on the studies carried out by Oliz et al.1 A mapping of the power distribution (W) was carried out inside the microwave oven, as described by Rosini et al.2 in order to decompose a larger number of samples simultaneously. Sausage samples were acquired in a local supermarket of Pelotas and were comminuted using a blender. The best conditions for micro digestion (mass, irradiation time, acid volume and microwave power) were optimized by employing a central composite design (CCD), at two levels.3 This way, 40 mg of sausage were weighed directly into mini vessels and was added 400 µL of HNO3. Then, the vessels were closed and placed in the microwave oven, using a rounded support with a capacity for six vessels. A beaker with deionized water was placed in the center of the support. The decomposition occurred in 3 min at level 7 (power of 475 W). The resulting solutions were transferred to polypropylene tubes and the final volume of 5.0 mL was completed with deionized water. The accuracy was evaluated through the analysis of certified reference material (SRM 1546 - meat homogenate) with good recoveries (80 to 117%) for all analytes. The method was applied for the analysis of a sausage sample. Sodium presented highest concentration (9108 ± 673 mg kg-1 ), followed by K (1364 ± 99 mg kg-1 ), Ca (604 ± 13 mg kg-1 ) and Mg (216 ± 19 mg kg-1 ). The analytes Cu, Fe and Zn presented close concentrations: 10 ± 0.8; 12 ± 0.7 and 12 ± 0.9 mg kg-1 , respectively. As conclusion, it was possible to perform simultaneous decomposition of the sausage samples using the sample treatment in micro-scale and the microwave oven, which provided an increase in the analytical frequency of the method. The procedure showed to be fast, safe and with lower consumption of reagents and samples, minimizing waste generation and the conventional microwave oven is easy to access, facilitating its use in routine analyzes.
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