This work has developed a miniaturized method based on matrix solid phase dispersion (MSPD) using C18 as dispersant and acetonitrile-water as eluting solvent for the analysis of legislated organochlorinated pesticides (OCPs) and polybrominated diphenylethers (PBDEs) in biota samples by GC with electron capture (GC-ECD). The method has compared Florisil-acidic Silica and C18 as dispersant for samples as well as different solvents. Recovery studies showed that the combination of C18-Florisil was better when using low amount of samples (0.1 g) and with low volumes of acetonitrile-water (2.6 mL). The use of SPME for extracting the analytes from the solvent mixture before the injection resulted in detection limits between 0.3 and 7.0 microg kg(-1) (expressed as wet mass). The miniaturized procedure was easier, faster, less time consuming than the conventional procedure and reduces the amounts of sample, dispersant and solvent volume by approximately 10 times. The proposed procedure was applied to analyse several biota samples from different parts of the Comunidad Valenciana.