The overall SPME–GC–MS procedure allowed us to determine several organochlorine, organophosphorus, fugicide, pyrethroid and organonitrogen pesticides simultaneously in plasma leading to low detection limits for most of the pesticides studied (0.02–1.0 µg/ ml ). The method can be suitable for detecting pesticides of different physico-chemical characteristics in exposed and non-exposed population and can be widened to the analysis of plasma samples.