RESUMEN
A method has been developed to determine 10 elements in Brazilian red wines using high-resolution continuum source flame atomic absorption spectrometry, a technique that allows the fast sequential determination of an essentially unlimited number of elements per sample, each one under previously optimized conditions. All measurements were made without sample preparation, using aqueous standard solutions for calibration. The results were in agreement within 99% of confidence (t-test) with those obtained by inductively coupled plasma optical emission spectrometry. The same grape, Cabernet sauvignon, was used in all experiments, and the wines from each region were prepared especially for this investigation in order to avoid any confusion due to grapes from other regions, which are often used in commercial wines. The elements K, Mn, Rb and Sr were found to be the best indicators for the origin of the wines, based on a Principal Component Analysis.
Asunto(s)
Manganeso/análisis , Potasio/análisis , Rubidio/análisis , Espectrofotometría Atómica/métodos , Estroncio/análisis , Vino/análisis , Brasil , Geografía , Análisis de Componente Principal , Especificidad de la Especie , Espectrofotometría Atómica/instrumentación , Vitis/química , Vitis/clasificaciónRESUMEN
Two analytical methods for the determination of cadmium in wheat flour by electrothermal atomic absorption spectrometry without prior sample digestion have been compared: direct solid sampling analysis (SS) and slurry sampling (SlS). Besides the conventional modifier mixture of palladium and magnesium nitrates (10 microg Pd+3 microg Mg), 0.05% (v/v) Triton X-100 has been added to improve the penetration of the modifier solution into the solid sample, and 0.1% H(2)O(2) in order to promote an in situ digestion for SS. For SlS, 30 microg Pd, 12 microg Mg and 0.05% (v/v) Triton X-100 have been used as the modifier mixture. Under these conditions, and using a pyrolysis temperature of 800 degrees C, essentially no background absorption was observed with an atomization temperature of 1600 degrees C. About 2 mg of sample have been typically used for SS, although as much as 3-5 mg could have been introduced. In the case of SlS multiple injections had to be used to achieve the sensitivity required for this determination. Calibration against aqueous standards was feasible for both methods. The characteristic mass obtained with SS was 0.6 pg, and that with SlS was 1.0 pg. The limits of detection were 0.4 and 0.7 ng g(-1), the limits of quantification were 1.3 and 2.3 ng g(-1) and the relative standard deviation (n=5) was 6-16% and 9-23% for SS and SlS, respectively. The accuracy was confirmed by the analysis of certified reference materials. The two methods were applied for the determination of cadmium in six wheat flour samples acquired in supermarkets of different Brazilian cities. The cadmium content varied between 8.9+/-0.5 and 13+/-2 ng g(-1) (n=5). Direct SS gave results similar to those obtained with SlS using multi-injections; the values of both techniques showed no statistically significant difference at the 95% confidence level. Direct SS was finally adopted as the method of choice, due to its greater simplicity, the faster speed of analysis and the better figures of merit.