Copper oxide was incorporated into MCM-41 by a one-pot synthesis under acidic conditions to prepare a new mesoporous nitrosamines trap for protection of the environment. The resulting composites were characterized by XRD, N2 adsorption-desorption, and H2 temperature-programmed reduction techniques, and their adsorption capabilities were assessed in the gaseous adsorption of N-nitrosopyrrolidine (NPYR). The adsorption isotherms were consistent with the Freundlich equation. The copper salt was deposited onto MCM-41 during the evaporation stage and was fixed on the host in the calcination process that followed. MCM-41 was able to capture NPYR in air below 373 K but not at 453 K. Loading of copper oxide on MCM-41 greatly improved its adsorption capability at elevated temperatures. The influence of the incorporation of copper into MCM-41 samples and the adsorption behavior of these samples are discussed in detail.