Evaluation of the extraction time, the time required to reach equilibrium in the fiber stationary phase, the plasma samples and the pesticides was evaluated through headspace extractions at 70 ◦C for 10, 20, 30, 40, 50 and 60 min. It was observed that the analytical signal for most of the compounds was enhanced for times up to 40 min. This time was therefore selected, since on average it represents the best condition for the set under study.