<p>A study was conducted to validate the gas chromatography-triple quadrupole mass spectrometry (GC-QqQ-MS) method as a cost-effective method for the analysis of polychlorinated dibenzo-p-dioxins/dibenzofurans (PCDD/Fs) in sediment samples. The instrument sensitivity for 17 PCDD/Fs congeners was determined to be in the range of 0.201 to 1.45&#xa0;ng/mL. The four-point calibration curve exhibited high linearity, with the mean relative response factors (RRFs) for PCDD/Fs ranging from 0.81 to 1.88, and RSD &lt; 20% met the analytical requirements of the standard method for gas chromatography combined with high-resolution mass spectrometry (GC-HRMS). The quantification limit of PCDD/Fs in sediments analyzed by the GC-QqQ-MS method was demonstrated to be 2 to 21 times higher than that of the GC-HRMS method. The results of PCDD/Fs concentration analysis in sediment matrix for 1 certified reference material sample, 3 international proficiency test samples, and 29 marine sediment samples between the two analytical methods showed a relatively good agreement, with a relative difference of ± 25%. Furthermore, the gas chromatography method using triple quadrupole mass spectrometry can be regarded as a viable alternative to high-resolution mass spectrometry for sediment samples with total mass concentrations of PCDD/Fs in the 500–1000&#xa0;pg/g range, and especially areas at risk of PCDD/Fs contamination.</p> Graphical Abstract <p></p>