Bioluminescence is widely distributed in various microorganisms, insects, shrimps, squid and fish. Bioluminescence can be also used as a reliable reporter for the assessment or monitoring of various aquatic samples containing toxicants such as pesticides, polychlorinated Biphenyls (PCBs), polyaromatic hydrocarbons, fuels, and heavy metals. In this study, luciferase were cultured from squid. Structured molecular films of adsorbed luciferase have been fabricated by means of a modified LB method using organo-modified clay. Chemisorption of luciferase to the anionic montmorillonite (MMT) surface was confirmed by a comparison between infrared spectra of multilayers of organo-clay and of chemisorbed luciferase. The bands of v C=O and δ N-H of luciferase were clearly identified in the spectra of multilayers coated with chemisorbed biomolecules. Luminescence spectra of buffer solution containing luciferase and multilayers of clay/luciferase suggest that enzyme activity were maintained in the case of multilayers of clay/luciferase.