A method to determine 8 polychlorinated biphenyls (PCBs), 23 organochlorine pesticides (OCPs) and 16 polycyclic aromatic hydrocarbons (PAHs) was described using dispersive liquid-liquid microextraction (DLLME) of a small amount of plasma or serum sample and gas chromatography-tandem mass spectrometry (GC-MS/MS).The appropriate selection of the extraction solvent and dispersing solvent contributes to a high extraction yield and a clean extract. To verify the developed method, the interference, linearity of the calibration curve, detection limit, precision and accuracy were evaluated. The calibration curves were linear by 2-3 orders of magnitude with correlation coefficients above 0.997 in all cases. The LODs of PCBs, OCPs and PAHs were measured in the ranges of 0.0006-0.0029, 0.001-0.029 and 0.0002-0.012 ng/mL. The intraday precision achieved by this method was 2.19-10.3% (PCBs), 1.65-14.3% (OCPs) and 0.91-12.8% (PAHs), and the intraday accuracy 1.56-7.37% (PCBs), 2.34-19.6% (OCPs) and 1.49-15.7% (PAHs). The advantage of this method is that the analysis of PCBs, OCPs, and PAHs can be performed in a single chromatographic run, and the low detection limit enables monitoring of target substances in low exposure general public samples, and the analysis procedure is relatively simple and fast.