The present investigation demonstrates establishment of United Nations Environment Programme (UNEP) priority Persistent Organic Pollutants (POPs) using high-resolution gas chromatography-high-resolution mass spectrometry. Particularly, POPs analytical methods were established using native and (13)C-labeled internal standards of HCHs, HCB, cyclodienes, chlordanes, DDTs, mirex, dioxin-like PCBs, PCDDs, and PCDFs by isotope dilution technique. The relative response factor for 6-point calibration curve native standards (18 replicate analysis) were in the ranges of 0.93-1.43 with relative standard deviation ranges from 1.68 to 4.96%. Instrument detection limit and instrument quantification limit was established for various POPs at femtograms. Concentrations of UNEP-POPs were measured in liver (n = 10) and egg (n = 10) of great cormorants and their major diet, gizzard shad (n = 2), collected in and around Tokyo, Japan. DDTs (ranges in liver and egg, respectively) were predominant accumulants (9800-310,000 and 9600-73,000) followed by dioxin-like PCBs (4500-69,000 and 7900-150,000), chlordanes (2600-16,000 and 700-4,800), cyclodienes (650-4600 and <1-1000), HCB (680-2800 and 180-590), HCHs (230-1800 and 120-490), PCDD/DFs (3.2-27 and 1.7-5.7) on nanogram per gram lipid basis. Concentrations (ranges) of POPs in gizzard shad were in the following order: DDTs (3900-16,000), chlordanes (3400-14,000), cyclodienes (340-1300), HCB (110-480), and HCHs (140-360) on nanogram per gram lipid basis.