This work presents a hyperspectral reflectance dataset of macroplastic samples. Samples analyzed consisted of pristine, artificially weathered and biofouled plastic specimens, and field samples collected in the docks of the Port of Antwerp and from the river Scheldt, near Temse Bridge (Belgium). The hyperspectral signal was measured in controlled conditions in an optical calibration facility, and, for a set of plastic specimens in a mesocosm setting that mimicked environmentally relevant concentrations of microalgae, changing levels of dissolved sediment or clear water. All the hyperspectral measurements were obtained using an Analytical Spectral Devices FieldSpec 4. The instrument was equipped with a 8° field of view at the calibration facility, while a 1° field of view was used in the mesocosm setting.