ABSTRACT: Here, a highly efficient membrane based on electrospun polycyclodextrin (poly-CD) nanofibers was prepared and exploited for the scavenging of various polycyclic aromatic hydrocarbons (PAHs) and heavy metals from water. The poly-CD nanofibers were produced by the electrospinning of CD molecules in the presence of a cross-linker (i.e., 1,2,3,4-butanetetracarboxylic acid), followed by heat treatment to obtain an insoluble poly-CD nanofibrous membrane. The membrane was used for the removal of several PAH compounds (i.e., acenaphthene, fluorene, fluoranthene, phenanthrene, and pyrene) and heavy metals (i.e., Pb2+, Ni2+, Mn2+, Cd2+, Zn2+, and Cu2+) from water over time. Experiments were made on the batch sorption of PAHs and heavy metals from contaminated water to explore the binding affinity of PAHs and heavy metals to the poly-CD membrane. The equilibrium sorption capacity (q e) of the poly-CD nanofibrous membrane was found to be 0.43 ± 0.045 mg/g for PAHs and 4.54 ± 0.063 mg/g for heavy metals, and the sorption kinetics fitted well with the pseudo-second-order model for both types of pollutants. The membrane could be recycled after treatment with acetonitrile or a 2% nitric acid solution and reused up to four times with similar performance. Further, dead-end filtration experiments showed that the PAH removal efficiencies were as high as 92.6 ± 1.6 and 89.9 ± 4.8% in 40 s for the solutions of 400 and 600 ?g/L PAHs, respectively. On the other hand, the removal efficiencies for heavy metals during the filtration were 94.3 ± 5.3 and 72.4 ± 23.4% for 10 and 50 mg/L solutions, respectively, suggesting rapid and efficient filtration of heavy metals and PAHs by the nanofibrous poly-CD membrane.