Because of the toxicity of polycyclic aromatic hydrocarbons (PAHs) and nitrated polycyclic aromatic hydrocarbons NPAHs), determination of their concentrations was of great interest in terms of soil and water pollution control. In this work, twelve surface soil samples were collected in every of 5 kmx5 km squares in Jiaxing city, Zhejiang province, China. Normal solid phase extraction was used for extraction of selected PAHs and NPAHs. A procedure for simultaneous determination of PAHs and NPAHs, including extraction, preseparation, reduction and analysis with HPLC, was developed. In the experiment, sixteen PAHs and fifteen NPAHs were detected from the samples of urban surface soil. PAR total concentrations ranged from 17.23 to 471.34 pg/g, while NPAH total concentrations ranged from 22.7 to 129.0 pg/g. Fluoranthene (11%), pyrene (11%), and benzo(a) anthracene (24%) were the main components of PAHs, while 2-nitrofluoranthene (14.3%) and 6-nitrochrysene (26.5%) were the most abundant components of NPAHs. Source analysis revealed that the PAHs originated from coal combustion around the study area, while NPAH studies suggested that primary emission of gasoline engines and daytime OH reactions were the dominant sources of these compounds.