A method for multi-residue screening of pesticide in aqueous sample was developed using sequential stir bar sorptive extraction and thermal desorption-comprehensive two-dimensional GC-time-of-flight mass spectrometry (Sequential SBSE-TD-GC × GC-TOF MS).Recovery of 83 pesticides-organochlorine, carbamate, organophosphorous, pyrethroid, and others-for SBSE, SBSE with salt addition (30% NaCl), and sequential SBSE was evaluated as a function of octanol-water distribution constant (Kow).Sequential SBSE consists of a SBSE performed sequentially on respectively a 5-mL sample without modifier and a 5-mL sample containing 30% NaCl.First extraction without modifier is mainly targeting solutes with medium and high Kow (LogKow > 3.5), second extraction with modified sample solution (containing 30% NaGl) is targeting solutes with low Kow (LogKow < 3.5).