Analysis of pesticide residues in seaweeds using matrix solid-phase dispersion and gas chromatography–mass spectrometry detection

Products containing organophosphates, carbamates and pyrethroids pesticides, employed as chemotherapeutants in aquaculture, can remain as residues in the marine environment. Matrix solid-phase dispersion (MSPD) was developed to extract seventeen pesticides from seaweed samples using Florisil and graphitized carbon black as clean-up adsorbents prior to gas chromatography–mass spectrometry (GC–MS) determination. The extraction has been optimised by a Box–Behnken design. The optimal conditions were 1 g of seaweed sample, 4 g of anhydrous sodium sulphate as dispersant, 3.6 g of Florisil and 0.4 g of GCB and an elution volume of 14 mL of a hexane:ethyl acetate mixture containing 40% ethyl acetate. The recoveries ranged from 81.6% to 113.2% with relative standard deviations (RSDs) ranging from 1.6% to 13.2%. The limits of detection (LOD) ranged from 0.5 to 2.9 ngg−1. Internal quality control was successfully carried out to verify the quality of the data obtained in the analysis of these pesticides in seaweed samples.