A method based on matrix solid-phase dispersion (MSPD) and gas chromatography-mass spectrometry
to determine pesticides in fish liver and crab hepatopancreas was optimized. Ethyl acetate and
acetonitrile were evaluated as elution solvents and their volumes were also checked. The best results were obtained with 1.0 g reused C18 as sorbent, using 5 mL acetonitrile as the elution solvent. Analytical recoveries ranged between 57 and 107% with RSD lower than 26% in fish liver and between 56 and 122% with RSD lower than 21% in crab hepatopancreas. The LOQ values for these compounds ranged from 0.05 to 0.5 mg kg−1 for crab hepatopancreas and from 0.125 to 1.25 mg kg−1 for fish liver. MPSD was shown to be easy and fast to use, with a clear advantage regarding costs because it does not need any expensive instrument. The proposed method was successfully applied to determine dimethoate, atrazine,clomazone, fenitrothion, malathion, fipronil and tebuconazole in fish liver and crab hepatopancreas samples.