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.
The extraction of pesticides lindane, heptachlor, aldrin, dieldrin and endrin from milk by HS-SPME was investigated followed by separation/detection of these compounds by GC-ECD.
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