The vertical and horizontal distribution of NPEOn and their metabolites of NP and NPEnC in the Upper Nansi Lake, North China were investigated using LC-MS and LC-MS/MS methods, sampling at three sites (St.1, St.2 and St.3) along the water flow direction. The total content of NPEOn (n=1–15) bound onto the sediment of this lake changed in the range of 60.7–631.5 μg/kg-dry with the horizontal flow direction and the vertical direction of the sediment cores with sediment thickness up to 35 cm. Compared to the presence levels of all detected NPEOn species, the content of NP was much higher, falling in 26.5–1,998.4 μg/kg-dry. A general increasing trend of the NP content along the water flow direction of this lake was revealed. NPEnC showed a roughly increasing trend from the upstream to the downstream, with the total concentrations being obviously lower than NPEOn and NP and falling in 2.13–23.1 μg/kg-dry. The short chain NPEOn dominant in NPEO mixtures in these sedimentary cores indicated that this lake received some effluents from STPs, and the sewage treatment ratio is relatively low in this area. Furthermore, the computed magnitudes of NPEO 1-2/NPEO1-15, NP/NPEO 1-15 and NPEC 1-10/NPEO 1-15 suggested that the non-oxidative hydrolytic transformation seemed to be a major process occurring within the sediment phase of Nansi Lake, while the oxidative hydrolytic transformation pathway was probably less involved.