In this study a new method for determination of cadmium in alcohol fuel using Moringa oleifera seeds as a biosorbent in an on-line preconcentration system coupled to flame atomic absorption spectrometry (FAAS) was developed. Flow and chemical variables of the proposed system were optimized through multivariate designs. The limit of detection for cadmium was 5.50microg L(-1) and the precision was below 2.3% (35.0microg L(-1), n=9). The analytical curve was linear from 5 to 150microg L(-1), with a correlation coefficient of 0.9993. The developed method was successfully applied to spiked alcohol fuel, and accuracy was assessed through recovery tests, with recovery ranging from 97.50 to 100%.
In this study, the experimental extraction conditions on applying headspace solid-phase microextraction and cold fiber headspace solid-phase microextraction (CF-HS-SPME) procedures to samples of six medicinal herbs commonly found in southern Brazil were optimized. The optimized conditions for headspace solid-phase microextraction were found to be an extraction temperature of 60°C and extraction time of 40 min. For CF-HS-SPME, the corresponding values were 60°C and 15 min. In the case of the coating temperature for the CF-HS-SPME system, two approaches were investigated: (i) Temperature of 5°C applied during the whole extraction procedure; and (ii) the use of two fiber temperatures in the same extraction procedure with the aim of extracting the volatile and semivolatile compounds, the ideal condition being 60°C for the first 7.5 min and 5°C for the final 7.5 min. The three extraction procedures were compared. The CF-HS-SPME procedure had good performance only for the more volatile compounds whereas the strategy using two coating temperatures in the same procedure showed good performance for all compounds studied. It was also possible to determine the profile for the volatile fraction of each herb studied applying this technique followed by GC-MS.
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