Abstract: Persistent organic pollutants (POPs) are closely related to the environment and human health and kept concerned by researchers at home and abroad. This study takes new POPs hexabromocyclododecanes and POP-like pollutants polycyclic aromatic hydrocarbons (PAHs) as research objects. A total of 18 dissolved PAHs and 3 HBCDs were collected and analyzed from the surface water of the Jiulongjiang Estuary in January and February, 2019. The results showed that the concentrations of dissolved PAHs in surface water ranged from 38.49 ng/L to 256.00 ng/L, and the concentrations of HBCDs ranged from ND to 49.951 ng/L. The highest concentrations of PAHs were recorded in compounds with two and three rings, but the lowest ones with five rings or above. The major source of PAHs was petroleum, mainly from the combustion of fossil fuels. Most of HBCDs detected were α-HBCD, followed by γ-HBCD and the least was β-HBCD. Compared with other domestic and foreign bays, rivers and basins, the PAH concentration in Jiulongjiang Estuary was still at a high level in contrast to the relatively low level of HBCD concentration.