The performance of powdered zeolite (PZ) adsorption/ultrafiltration (UF) with real secondary effluents is investigated. With the assistance of PZs, the membrane fouling rate was reduced and the permeate flux recovery as well as the advanced treatment of the secondary effluents were enhanced. 3D excitation emission matrix (3D-EEM) fluorescence spectra indicate that the removal of fluorescence intensity for aromatic proteins, fulvic acid-like materials, soluble microbial by-product-like materials, and humic acid-like organics could be improved by PZs. UF membranes with PZs can increase the removal efficiency of organics, especially of those with low molecular weight. The characteristics of the cake layer on the surface of an UF membrane were determined by scanning electron microscopy and electron energy-dispersive X-ray spectroscopy for the combined adsorption/UF membrane.