Meconium is the earliest stool of newborns. It is a complex matrix that reflects the degree of fetal exposure to environmental pollutants. To investigate exposure to xenobiotics, an analytical method was developed to identify and quantify some pesticides and their metabolites and BTEX metabolites in meconium. Samples were prepared by two liquid-solid extractions and purified twice using SPE cartridges, followed by analysis with liquid chromatography coupled with tandem mass spectrometry. SPE cartridges (polymeric phase with hydrophilic and hydrophobic interactions, ion exchange, mixed mode) were tested and matrix effects were evaluated to determine purification performance. The quantification limits in meconium of this multi-residue method were in the range of 30 ng g(-1). The analytical method was applied to "real" meconium samples. Some target analytes were determined in most samples.