Release assessment of organo-modified montmorillonite (O-MMT) nanoclay and the organo-modifiers (surfactants) was performed on two types of polymer–clay nanocomposites: polypropylene (PP) and polyamide 6 (PA6) with O-MMT. In accordance with ASTM D4754-11, nanocomposite films were exposed to ethanol as a fatty-food simulant at 70 °C. The release of O-MMT, with Si and Al used as the nanoclay markers, was evaluated by graphite furnace atomic absorption spectrometry. The nanoclay particles released in ethanol were visualized by transmission electron microscopy (TEM). More nanoclay particles were released from PP–clay films (0.15 mg L(–1)) than from PA6–clay films (0.10 mg L(–1)), possibly due to the lack of interaction between the nanoclay and PP as indicated by the structure and morphology in the TEM images. The surfactant release was quantified by a liquid chromatography tandem mass spectrometry (LC-MS/MS) method. A substantial amount of surfactant was released into ethanol (3.5 mg L(–1) from PP–clay films and 16.2 mg L(–1) from PA6–clay films), indicating changes in the nanoclay structure within the nanocomposite while it was exposed to ethanol. This research has provided information for the determination of exposure doses of nanoclay and surfactant in biosystems and the environment, which enabled the risk assessment.