Trace residues of organochlorine pesticides (OCPs) in estuarine surface sediments were investigated at three protected wetlands in southern Taiwan using high‐resolution gas chromatography/high‐resolution mass spectrometry (HRGC/HRMS) and gas chromatography‐electron capture detector (GC‐ECD). This study facilitates the development of new strategies for investigating OCPs, particularly at background levels. Linear relationships were obtained between total OCP concentrations (∑OCP), as analyzed by HRGC/HRMS, and the sediment's total organic carbon (TOC) and water content. It contrasted with the results acquired by GC‐ECD, where no significant relationship was found. GC‐ECD is a rugged option for daily routine practice, particularly in cases of patterns yielded by GC‐ECD is clear; the HRGC/HRMS method provides more reliable qualitative and quantitative capabilities and is highly recommended for studying the fate of OCPs and carrying out risk assessments. The average ∑OCP of these three wetlands by HRGC/HRMS was found in a range of 0.214 to 1.049 ng/g dry weight. The highest OCP level might be attributed to associated irrigation systems receiving massive discharges of domestic sewage from an urban area upstream of the wetland. The ratio of dichlorodiphenyltrichloroethane (DDT) to its metabolites indicated that the DDT residue in these areas was from aged input. According to sediment quality guidelines, adverse ecotoxicological effects of OCPs upon sediments were not expected in these protected wetlands.
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